CN1612960A - Process for treating a lipophilic fluid - Google Patents

Abstract

The present invention relates to a process for treating a lipophilic fluid contained in an emulsion of water and lipophilic fluid. The process includes the steps of pretreating the emulsion, removing lipophilic fluid from the emulsion, and purifying the lipophilic fluid to remove at least a portion of the impurities collected during the use of the emulsion. Method options are provided for each of the aforementioned steps.

Description

Method for processing lipophilic fluid

field of invention

The present invention relates to a method for treating a lipophilic fluid contained in an emulsion of water and a lipophilic fluid. The method includes the steps of pre-treating the emulsion and removing lipophilic fluid from the emulsion and purifying the lipophilic fluid to remove at least some of the impurities collected during use of the emulsion. The present invention provides method options for each of the preceding steps.

Background of the invention

Traditional laundering techniques for cleaning and caring for fabric articles such as clothing have long included traditional water-based washing and techniques commonly referred to as "dry cleaning". Traditional water-based laundering techniques involve immersing fabric articles in a solution of water and detergent or soap products, followed by rinsing and drying. However, this traditional immersion cleaning technique has proven unsatisfactory for a wide range of fabric items that require special care and/or cleaning methods due to fabric content, construction, etc., and are not suitable for immersion in water .

Accordingly, the use of "dry cleaning" washing methods has been developed. Dry cleaning typically involves the use of non-aqueous, lipophilic fluids as solvents or solutions for cleaning. In this regard, fabrics that are incompatible with water immersion can be cleaned and cared for without the potentially damaging side effects that water can bring.

Although a wide range of non-aqueous lipophilic fluids are available, many require small amounts of water in the form of emulsions or microemulsions to maximize cleaning effectiveness without sacrificing the "safety" imparted to fabrics by dry cleaning. Furthermore, it is desirable to reuse and/or purify non-aqueous lipophilic fluids to reduce the higher running costs associated with dry cleaning compared to water-based washing. Reuse of lipophilic fluids can pose particular challenges when water, dirt and body soil are also present in the emulsion after its use. However, reuse poses special problems, especially when there are equipment space, cost, and safety concerns. Therefore, there is a need for a cost-effective, efficient and safe method to treat or purify lipophilic fluids after their use, especially when water and adjuncts such as emulsifiers are used.

Conventional separation techniques for dry cleaning solvent/water emulsions and/or mixtures typically involve distillation of all solvent-containing fluids, including those that do not require distillation. In this respect, distillation is used not only to remove impurities such as body soil from dry cleaning solvents after use, but also to separate the solvent from water - a function that can be achieved in other ways. Distillation often involves high operating costs in the form of energy and equipment necessary to obtain the separation, and is therefore not advisable in many cases, especially when the equipment is in the consumer's home. Finally, as mentioned above, distillation is not necessary for all solvent-containing fluids produced by dry cleaning. For example, evaporatively dried solvent-water mixtures do not necessarily require distillation, since they are essentially free of impurities, requiring only a water-solvent separation operation.

Accordingly, cost-effective, efficient and safe methods are needed to dispose of lipophilic fluids after use, especially when water and emulsifiers are present.

Summary of the invention

The present invention provides methods for disposing of post-use lipophilic fluids in a cost-effective, efficient and safe manner.

In a first embodiment, the present invention provides a method of treating a lipophilic fluid contained in an emulsion of water and at least one lipophilic fluid. The method has three main steps: pretreatment of the emulsion, recovery of the lipophilic fluid from the emulsion, and purification of the lipophilic fluid.

In a second embodiment, the present invention provides methods for purifying lipophilic fluids and lipophilic fluid vapors. The method comprises collecting a lipophilic fluid vapor and a first emulsion containing water and a lipophilic fluid, condensing the lipophilic fluid vapor, combining the condensed lipophilic fluid vapor with the first emulsion to form a second emulsion, pretreating the second emulsion , recovering the lipophilic fluid from the second emulsion and purifying the lipophilic fluid.

These and other aspects, features and advantages of the present invention will become apparent to those of ordinary skill in the art from the following detailed description and appended claims. All percentages, ratios and proportions stated herein are by weight unless otherwise specified. Unless otherwise indicated, temperatures stated herein are in degrees Celsius (° C.). All measurements are in SI units unless otherwise indicated. All cited documents are incorporated by reference in their respective sections.

Detailed description of the invention

definition

The term "lipophilic fluid" as used herein is intended to include any non-aqueous fluid or vapor capable of removing sebum, as defined in the test described below.

As used herein, the term "fabric article" refers to any article that is normally cleaned by conventional laundering or dry cleaning methods. Likewise, the term includes articles of clothing, linen, drapes and clothing accessories. The term also includes other articles made wholly or partly of fabric, such as tote bags, furniture covers, tarpaulins, and the like.

As used herein, the term "absorbent material" or "absorbent polymer" refers to any material capable of selectively absorbing or absorbing water and/or aqueous liquids without absorbing lipophilic fluids, as will be described in more detail. In other words, the absorbent material or absorbent polymer includes a water absorbent. In this field, they may also refer to "responsive gels", "gels" and "polymeric gels". For many phase transition gels, see the textbook "Responsive Gels, Volume Transitions" II, Ed K. Dusek, Springer Verlag Berlin, 1993 (this document is incorporated herein by reference). See also "Thermo-responsive Gels", Radiat. Phys. Chem., Volume 46, No. 2, pp. 185-190, Elsevier Science Ltd. Great Britain, 1995 (which is incorporated herein by reference). Superabsorbent polymers also suitable for use in the present invention are absorbent materials having an absorbent capacity equal to or higher than 5 g/g. See also "Superabsorbent Polymers Science and Technology", edited by Fredric L. Buchholz and Nicholas A. Peppas, American Chemical Society, Washington DC, 1994 (especially Chapter 9, by Tadao Shimomura and Takashi Namba, entitled "Preparation and Application of High- Performance Superabsorbent Polymers"), which is incorporated herein by reference.

As used herein, the term "absorbent matrix permeability aid" or "barrier material" or "separator" refers to any fibrous or particulate material that is at most only slightly soluble in water and/or lipophilic fluids.

As used herein, the term "absorbent substrate" refers to any form of substrate capable of absorbing and/or absorbing water. At least, it includes absorbent material. It may optionally include barrier materials and/or high surface area materials.

lipophilic fluid

The lipophilic fluid herein is a fluid that is in the liquid phase under the operating conditions of the fabric article care appliance, in other words, during care of the fabric article according to the present invention. Generally, the lipophilic fluid can be completely liquid at ambient temperature and pressure, or it can be a fusible solid, for example, a substance that becomes liquid in the temperature range of about 0°C to about 60°C, or can be Mixtures of liquid and vapor phases at ambient temperature and pressure (eg, 25° C. and a pressure of 1 atmosphere) are included. Thus, the lipophilic fluid is not a compressible gas such as carbon dioxide.

Preferably, the lipophilic fluids of the present invention are non-flammable or have relatively high flash point and/or low VOC (volatile organic compound) properties equal to or preferably exceeding those of known conventional dry cleaning fluids for use in the dry cleaning industry These terms have their ordinary meanings.

Furthermore, suitable lipophilic fluids for the present invention are flowable and non-viscous fluids.

In general, the lipophilic fluid of the present invention must be a fluid capable of at least partially dissolving sebum or body soil as described in the tests below. Mixtures of lipophilic fluids are also suitable and, provided the lipophilic fluid test requirements described below are met, the lipophilic fluid may include any fraction of dry cleaning solvents, particularly those that include fluorinated solvents or perfluorinated amines. Newer types of dry cleaning solvents. Some perfluorinated amines, such as perfluorotributylamine, although not suitable for use as lipophilic fluids, can be present as one of many possible adjuvants in compositions comprising lipophilic fluids.

Other suitable lipophilic fluids include, but are not limited to, diol solvent systems, e.g., higher diols such as C6- or C8- or higher diols, cyclic and acyclic types of silicone solvents, etc., and their mixture.

Preferred non-aqueous lipophilic fluids suitable for incorporation as a major component of the compositions of the present invention include low volatility non-fluorinated organics, silicones, especially those other than aminofunctional polysiloxanes, and mixtures thereof . Low volatility non-fluorinated organics include, for example, OLEAN ^(R) and other polyol esters, or certain relatively nonvolatile biodegradable medium chain branched petroleum fractions.

Other preferred non-aqueous lipophilic fluids suitable for incorporation as a major component of the compositions of the present invention include, but are not limited to, glycol ethers such as propylene glycol methyl ether, propylene glycol n-propyl ether, propylene glycol t-butyl ether, propylene glycol n-butyl ether, dipropylene glycol methyl ether, dipropylene glycol n-propyl ether, dipropylene glycol tert-butyl ether, dipropylene glycol n-butyl ether, tripropylene glycol methyl ether, tripropylene glycol n-propyl ether, tripropylene glycol tert-butyl ether, tripropylene glycol n-butyl ether. Silicones suitable for use as a major component of the composition (e.g., greater than 50% of the composition), including cyclopentasiloxane (sometimes referred to as "D5"), and/or silicones having about a similar volatility Type analogs, optionally, supplemented by other compatible siloxanes. Suitable polysiloxanes are well known in the literature, see, for example, "Encyclopedia of Chemical Technology" by Kirk Othmer, and are available from a number of commercial sources including General Electric, Toshiba Silicone, Bayer and Dow Corning. Other suitable lipophilic fluids are available from Procter & Gamble or Dow Chemical and other suppliers.

Identification of lipophilic fluid and lipophilic fluid test (LF test)

Any non-aqueous fluid that meets the known requirements of a dry cleaning fluid (eg, flash point, etc.) and at least partially dissolves sebum, as demonstrated by the test methods described below, is suitable for use as a lipophilic fluid in the present invention. As a general guideline, perfluorobutylamine (Fluorinert FC- ^43® ) by itself (with or without auxiliaries) is by definition a reference substance, which is not suitable for use as the lipophilic fluid of the present invention (which is essentially a non-solvent), whereas Cyclopentasiloxane has suitable sebum-dissolving properties and dissolves sebum.

The following is a method for investigating and identifying other materials, eg, other low viscosity, free-flowing silicones, as suitable for use as lipophilic fluids. The method used commercially available Crisco ⁽ R) canola oil, oleic acid (95% purity, from Sigma Aldrich Co.), and squalene (99% purity, from JT Baker) as model soils for sebum. During the evaluation, the test substance should be substantially anhydrous and free from any additional auxiliaries or other substances.

Prepare three vials, each containing one type of lipophilic soil. 1.0 g canola oil was placed in the first vial; 1.0 g oleic acid (95%) was placed in the second vial, and 1.0 g squalene (99.9%) was placed in the third and final vial . 1 g of the lipophilic fluid to be tested is added to each vial. Each vial containing lipophilic soil and fluid to be tested was mixed for 20 seconds on a standard vortex mixer at maximum setting at room temperature and pressure, respectively. Place the vial on the bench and keep at room temperature and pressure for 15 minutes. Upon standing, if a clear single phase forms in all vials containing lipophilic soil, the non-aqueous fluid qualifies as suitable as a "lipophilic fluid" according to the present invention. However, if two or more separate layers form in all three vials, further determination of the amount of non-aqueous fluid dissolved in the oil phase is required before rejecting or accepting the non-aqueous fluid as an acceptable substance .

In such cases, carefully withdraw 200 microliters of sample from each layer of each vial with a syringe. After determining the retention times for each of the calibration samples of the three model soils and fluids under test, the layer samples were syringed into GC autosampler vials and subjected to routine GC analysis. If, by GC, greater than 1%, preferably more, of the test fluid is found to be present in any layer consisting of oleic acid, canola oil, or squalene, then that test fluid also qualifies as a prophylaxis. fat fluid. If required, the method can be further calibrated using heptafluorotributylamine, ie, Fluorinert FC-43 (fail) and cyclopentasiloxane (pass). A suitable GC is a Hewlett Packard Gas Chromatograph HP5890 Series II equipped with split/splitless injector and FID. A suitable column for detecting the presence of lipophilic fluid is J&WScientific Capillary Column DB-1HT, 30 meters, 0.25mm inner diameter, 0.1um film thickness, catalog number 1221131. The GC is suitable for operation under the following conditions:

Carrier gas: hydrogen

Pre-column pressure: 9psi (62Kpa)

Flow: column flow @ ~ 1.5ml/min

  Split flow @～250-500ml/min

  Diaphragm purification flow@1ml/min

Injection: HP7673 automatic sampler, 10ul syringe, 1ul injection volume

Syringe temperature: 350°C

Detector temperature: 380°C

Oven heating program: initial temperature 60°C, keep for 1 minute

The rate is 25°C/min.

The final temperature is 380°C and kept for 30 minutes.

Preferred lipophilic fluids suitable for use in the present invention qualify for further use on the basis of having excellent laundry care characteristics. Garment care signature testing is well known in the art and involves testing the fluid to be identified using various garment or fabric article components, including elastomers used in fabrics, yarns, seams, etc., and various buttons. Preferred lipophilic fluids for use in the present invention have good garment care characteristics, eg they have good shrinkage and/or fabric crease characteristics and do not significantly damage plastic buttons. Certain substances that are acceptable for use as lipophilic fluids in terms of sebum removal, such as ethyl lactate, cannot be used due to their tendency to dissolve buttons, and if such substances are to be used in the composition of the present invention, they should be mixed with water and and/or other solvents formulated so that the entire mixture does not substantially damage the buttons. Other lipophilic fluids, such as D5, meet this laundry care need well. Some suitable lipophilic fluids are described in the following issued US Patents: 5,865,852, 5,942,007, 6,042,617, 6,042,618, 6,056,789, 6,059,845, and 6,063,135, all of which are incorporated herein by reference.

Lipophilic fluids may include linear and cyclic polysiloxanes, hydrocarbons and chlorinated hydrocarbons, excluding PERC and DF2000, which are expressly not lipophilic fluids as defined herein. More preferred are linear and cyclic polysiloxanes and hydrocarbons of the glycol ether, acetate, lactate family. Preferred lipophilic fluids include cyclic siloxanes having a boiling point below about 250°C at 760 mm Hg. Specifically preferred cyclic siloxanes for use in the present invention are octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane and dodecamethylcyclohexasiloxane. Preferably, the cyclic siloxane comprises decamethylcyclopentasiloxane (D5, pentamer) and is substantially free of octamethylcyclotetrasiloxane (tetramer) and dodecamethylcyclohexasiloxane Oxane (hexamer).

It should be understood, however, that useful cyclic siloxane mixtures may contain minor amounts of other cyclic siloxanes in addition to the preferred cyclic siloxanes.

The cyclic siloxanes include octamethylcyclotetrasiloxane and hexamethylcyclotrisiloxane or higher rings such as tetradecamethylcyclohexasiloxane. Generally, the amount of these other cyclic siloxanes that can be used in the cyclic silicone mixture is less than about ten percent by weight of the total mixture. The industry standard for cyclic siloxane mixtures is that the mixture includes less than about 1% octamethylcyclotetrasiloxane by weight of the mixture.

Accordingly, the lipophilic fluids of the present invention preferably comprise greater than about 50%, more preferably greater than about 75%, even more preferably at least about 90%, most preferably at least about 95% decamethylcyclopentasil by weight of the lipophilic fluid oxane. Alternatively, the lipophilic fluid may comprise a siloxane of a mixture of cyclic silicones having, by weight of the mixture, greater than about 50%, preferably greater than about 75%, more preferably at least about 90%, most preferably at least From about 95% up to about 100% decamethylcyclopentasiloxane, and less than about 10%, preferably less than about 5%, more preferably less than about 2%, even more preferably less than about 1%, most preferably from less than about 0.5% to about 0%, octamethylcyclotetrasiloxane and/or dodecamethylcyclohexasiloxane.

When present in the treatment composition according to the present invention, the content of lipophilic fluid is preferably from about 70% to about 99.99%, more preferably from about 90% to about 99.9%, and even more by weight of the treatment composition. Preferably from about 95% to about 99.8%.

When present in the consumable leather treatment/washing compositions according to the present invention, the lipophilic fluid is preferably present in an amount of from about 0.1% to about 90% by weight of the consumable leather treatment/washing composition, more preferably From about 0.5% to about 75%, and even more preferably from about 1% to about 50%.

Auxiliary ingredients

Auxiliary materials can vary widely and be used in widely varying levels. For example, detersive enzymes, such as proteases, amylases, cellulases, esterases, etc. and bleach catalysts, including macrocycles containing manganese or similar transition metals, are useful in washing and cleaning products and can be used in the present invention Use at typical or atypical levels. Catalytic auxiliary materials, such as enzymes, can be used in "forward" or "reverse" mode, which is a useful finding independently from the present invention. For example, esterases or other hydrolases are used to convert fatty acids to esters, optionally in the presence of alcohol as an aid, thereby increasing their solubility in lipophilic fluids. This is a "reverse" operation, in contrast to the normal use of this hydrolase in water, which converts less water soluble aliphatic esters into more water soluble species. In any event, any auxiliary ingredients must be suitable for use in combination with lipophilic fluids.

The composition may include an emulsifier. Emulsifiers are well known in the chemical arts. The basic function of an emulsifier is to make a stable or semi-stable emulsion of two or more insoluble or semi-dissolved phases. It is preferred in the claimed invention that the emulsifier serves a dual purpose, where it acts not only as an emulsifier but also as a handling performance enhancer. For example, the emulsifier may also act as a surfactant to promote cleaning performance. Both general emulsifiers and emulsifier/surfactants are commercially available.

Some suitable cleaning additives include, but are not limited to, builders, surfactants, enzymes, bleach activators, bleach catalysts, bleach boosters, bleaches, alkalinity sources, antimicrobials, colorants, fragrances, pro-fragrances, Finishing Aid, Lime Soap Dispersant, Composition Malodor Control Agent, Odor Neutralizer, Polymeric Dye Transfer Inhibitor, Crystal Growth Inhibitor, Photobleach, Heavy Metal Ion Sequestrant, Antitarnish Agent, Antimicrobial agents, antioxidants, anti-redeposition agents, dielectrics, pH modifiers, thickeners, abrasives, divalent or trivalent ions, metal ion salts, enzyme stabilizers, corrosion inhibitors, diamines or polyamines and/or or their alkoxylates, foam stabilizing polymers, solvents, processing aids, fabric softeners, optical brighteners, hydrotropes, defoamers, foam boosters, fabric softeners, antistatic agents, dye curing agents, dye wear inhibitors, anti-stain agents, wrinkle reducers, anti-wrinkle agents, soil release polymers, soil repellants, sunscreens, anti-stain agents, and mixtures thereof.

The term "surfactant" traditionally refers to a substance that is surface active in water, in a lipophilic fluid, or in a mixture of the two. Some exemplary surfactants include nonionic, cationic and silicone surfactants found in conventional aqueous detergent systems. Suitable nonionic surfactants include, but are not limited to:

a) polyethylene oxide condensates of nonylphenol and myristyl alcohol, as described in US Patent 4685930 Kasprzak; and

b) Fatty alcohol ethoxylates, R-(OCH ₂ CH ₂ ) _a OH a = 1 to 100, typically 12 to 40, R = hydrocarbon residue 8 to 20 carbon atoms, typically linear alkyl . Examples are: polyoxyethylene lauryl ether with 4 or 23 ethoxyl groups; polyoxyethylene cetyl ether with 2, 10 or 20 ethoxyl groups; polyoxyethylene cetyl ether with 2, 10, 20, 21 or Polyoxyethylene stearyl ether with 100 ethoxyethylene groups; polyoxyethylene (2), (10) oleyl ether with 2 or 10 oxyethylene groups. Commercially available examples include, but are not limited to: ALFONIC, BRIJ, GENAPOL, NEODOL, SURFONIC, TRYCOL. See also US Patent 6,013,683, Hill et al.

Suitable silicone-based surfactants include polyether siloxanes of the formula:

M _a D _b D′ _c D″ _d M′ _2-a

where a is 0 to 2; b is 0 to 1000; c is 0 to 50; d is 0 to 50, provided that a+c+d is at least 1;

M is R ¹ _3-e X _e SiO1/2, wherein R ¹ is independently H or a monovalent hydrocarbon group, X is a hydroxyl group, and e is 0 or 1;

M' is R ² ₃ SiO _1/2 , wherein R ² is independently H, a monovalent hydrocarbon group or (CH ₂ ) _f -(C ₆ H ₄ ) _g O-(C ₂ H ₄ O) _h -(C ₃ H ₆ O) _i -(C _k H _2k O) _j -R ³ , provided that at least one R ² is (CH ₂ ) _f -(C ₆ H ₄ ) _g O-(C ₂ H ₄ O) _h -( C ₃ H ₆ O) _i -(C _k H _2k O) _j -R ³ , wherein R ³ is independently H, a monovalent hydrocarbon group or an alkoxy group, f is 1 to 10, g is 0 or 1, h is 1 to 50, i is 0 to 50, j is 0 to 50, k is 4 to 8;

D is R ⁴ ₂ SiO _2/2 , wherein R ⁴ is independently H or a monovalent hydrocarbon group;

D' is R ⁵ ₂ SiO _2/2 , where R ⁵ is independently R ² , with the proviso that at least one R ⁵ is (CH ₂ ) _f -(C ₆ H ₄ ) _g O-(C ₂ H ₄ O) _h -(C ₃ H ₆ O) _i -(C _k H _2k O) _j -R ³ , wherein R ³ is independently H, a monovalent hydrocarbon group or an alkoxy group, f is 1 to 10, g is 0 or 1, h is 1 to 50, i is 0 to 50, j is 0 to 50, k is 4 to 8; and

D″ is R ⁶ ₂ SiO _2/2 , wherein R ⁶ is independently H, a monovalent hydrocarbon group, or (CH ₂ ) ₁ (C ₆ H ₄ ) _m (A) _n -[(L) _o -(A') _p- ] _q- (L') _r Z(G) _s , where 1 is 1 to 10; m is 0 or 1; n is 0 to 5; o is 0 to 3; p is 0 or 1; q is 0 to 10; r is 0 to 3; s is 0 to 3; C ₆ H ₄ is unsubstituted or substituted with C _1-10 alkyl or alkenyl; A and A' each independently represent ester, ketone, Ether, thiol, amido, amino, C _1-4 fluoroalkyl, C _1-4 fluoroalkenyl, branched or linear polyalkylene oxide, phosphate, sulfonyl, sulfuric acid Root, ammonium, and the connecting part of their mixture; L and L' are each independently C _1-30 straight chain or branched chain alkyl or alkenyl, or unsubstituted or substituted aryl; Z is hydrogen, Carboxylic acid, hydroxyl, phosphate (phosphato), phosphate, sulfonyl, sulfonate, sulfate, branched or linear polyalkylene oxide, nitroxyl, glyceryl, unsubstituted or with C _{1 -30} Alkyl or alkenyl substituted aryl, unsubstituted or carbohydrate substituted with C _1-10 alkyl or alkenyl or ammonium; G is an anion or cation, such as H ⁺ , Na ⁺ , Li ⁺ , K ⁺ , NH ⁴⁺ , Ca ⁺² , Mg ⁺² , Cl ^- , Br ^- , I ^- , mesylate or tosylate.

Examples of such silicone-based surfactants as described herein above can be found in EP-1,043,443A1, EP-1,041,189 and WO-01/34,706 (all to GE Silicones) and US Patent 5,676,705, US Patent 5,683,977, US Patent 5,683,473 and EP- -1,092,803A1 (all awarded to Lever Brother).

Commercially available, non-limiting examples of suitable silicone-based surfactants are TSF4446 (e.g., General Electric Silicones), XS69-B5476 (e.g., General Electric Silicones); Jenamine HSX (e.g., DelCon) and Y12147 (e.g., OSi Specialties).

Another preferred class of materials suitable for use in the surfactant component is of an organic nature. Preferred materials are organic sulfosuccinate surfactants having carbon chains of from about 6 to about 20 carbon atoms. Most preferred are organosulfosuccinates comprising dialkyl chains with carbon chains of from about 6 to about 20 carbon atoms per hydrocarbon chain. Also preferred are chains comprising aryl or alkylaryl, substituted or unsubstituted, branched or linear, saturated or unsaturated groups.

Commercially available, non-limiting examples of suitable organosulfosuccinate surfactants are available under the tradenames Aerosol OT and Aerosol TR-70 (eg, Cytec).

Another preferred class of surfactants are nonionic surfactants, especially those with low HLB values. Preferred nonionic surfactants have HLB values below about 10, more preferably below about 7.5, and most preferably below about 5. Preferred nonionic surfactants also have about 6 to 20 carbon atoms in the surfactant chain and about 1 to 15 ethylene oxide and/or propylene oxide units (i.e., C6 -20 EO/PO 1-15), preferably the nonionic surfactant is selected from those at C7-11, EO/PO 1-5 (i.e., C7-11 EO 2.5).

When present in the fabric care compositions of the present invention, the surfactant component preferably comprises from about 0.01% to about 10%, more preferably from about 0.02% to about 5%, even more preferably from about 0.05% to About 2% fabric care composition.

When present in the consumable detergent compositions of the present invention, the surfactant component preferably comprises from about 1% to about 99%, more preferably from 2% to about 75%, even more preferably from about 5% to about 99% by weight. About 60% of the detergent composition is consumable.

Suitable cationic surfactants include, but are not limited to, dialkyldimethylammonium salts of the formula:

R'R”N ⁺ (CH ₃ ) ₂ X ^-

wherein each R', R" is independently selected from 12 to 30 carbon atoms or derived from tallow, coconut oil or soybean, X=Cl or Br, examples include: didodecyldimethylammonium bromide (DDAB), Dihexadecyldimethylammonium chloride, Dihexadecyldimethylammonium bromide, Dioctadecyldimethylammonium chloride, Dieicosyldimethylammonium chloride Ammonium, Dibehenyldimethylammonium Chloride, Dicocotylmmonium Chloride, Ditallowdimethylammonium Bromide (DTAB). Commercially available examples include, but are not limited to: ADOGEN , ARQUAD, TOMAH, VARIQUAT. See also US Patent 6,013,683, Hill et al.

Suitable silicone surfactants include, but are not limited to, polyalkylene oxide polysiloxanes having the hydrophobic portion of dimethylpolysiloxane and one or more hydrophilic polyalkylene side chains, and has the following formula:

R ¹ -(CH ₃ ) ₂ SiO-[(CH ₃ ) ₂ SiO] _a -[(CH ₃ )(R ¹ )SiO] _b -Si(CH ₃ ) ₂ -R ¹

wherein a+b is from about 1 to about 50, preferably from about 3 to about 30, more preferably from about 10 to about 25, and each ^R is the same or different, and is selected from methyl and poly(ethylene oxide) having the formula alkane/propylene oxide) copolymer:

-(CH ₂ ) _n O(C ₂ H ₄ O) _c (C ₃ H ₆ O) _d R ²

At least ^one R is a poly(ethylene oxide/propylene oxide) copolymer, and wherein n is 3 or 4, preferably 3; and c (for all polyalkylene oxide side groups) has a value from 1 to about 100 , preferably from about 6 to about 100; and d is from 0 to about 14, preferably from 0 to about 3; and more preferably d is 0; and c+d has a value from about 5 to about 150, preferably from about 9 to about 100, per R ² are the same or different and are selected from hydrogen, alkyl and acetyl having 1 to 4 carbon atoms, preferably hydrogen and methyl. Examples of these surfactants can be found in US Patents 5,705,562 and 5,707,613, both issued to Hill.

An example of such a surfactant is Silwet ^(R) surfactant, available from CK Witco, OSi Division, Danbury, Connecticut. Representative Silwet surfactants are as follows.

name average molecular weight average of a+b average of sum of c

L-7608 600 1 9

L-7607 1,000 2 17

L-77 600 1 9

L-7605 6,000 20 99

L-7604 4,000 21 53

L-7600 4,000 11 68

L-7657 5,000 20 76

L-7602 3,000 20 29

The molecular weight (R ¹ ) of the polyalkyleneoxy groups is less than or equal to about 10,000. Preferably, the molecular weight of the polyalkyleneoxy groups is less than or equal to about 8,000, and most preferably in the range of about 300 to about 5,000. Accordingly, the values of c and d may be those numbers which provide molecular weights within these ranges. However, the number of ethyleneoxy units (—C ₂ H ₄ O)(R ¹ ) in the polyether chain must be sufficient to render the polyalkylene oxide polysiloxane water-dispersible or water-soluble. If propyleneoxy groups are present in the polyalkyleneoxy chain, they can be distributed randomly in the chain or be present in block form. Preferred Silwet surfactants are L-7600, L-7602, L-7604, L-7605, L-7657, and mixtures thereof. In addition to surface activity, polyalkylene oxide polysiloxane surfactants can also provide other benefits such as antistatic benefits and fabric softness.

The preparation of polyalkylene oxide polysiloxanes is well known in the art. The polyalkylene oxide polysiloxanes of the present invention can be prepared according to the procedure described in US Pat. No. 3,299,112. Another suitable silicone surfactant is SF-1488, which is commercially available from GE silicone fluids.

These or other surfactants suitable for use as auxiliaries in combination with lipophilic fluids are well known in the art and are described in more detail in "Encyclopedia of Chemical Technology" by Kirk Othmer, Third Edition, Vol. 22, 360-379, "Surfactants and Detersive Systems". Further suitable nonionic detergent surfactants are generally disclosed in US Patent 3,929,678, Laughlin et al., December 30, 1975, column 13, line 14 through column 16, line 6.

The auxiliary agent can also be an antistatic agent. Any suitable antistatic agent well known in the laundry and dry cleaning arts is suitable for use in the methods and compositions of the present invention. Particularly suitable as antistatic agents are fabric softeners known to provide antistatic benefits. For example, those softeners with fatty acyl groups whose iodine value is above 20, such as N,N-bis(tallowoyloxyethyl)-N,N-dimethylammonium methylsulfate. It should be understood, however, that the term "antistatic agent" should not be limited to only this subclass of fabric softeners, and includes all antistatic agents.

Although the methods and/or compositions employed in the present invention will be described in detail, it should be understood that any composition, method and/or apparatus capable of practicing the present invention will be appreciated by those skilled in the art.

absorbent material

The absorbent material of the present invention comprises one or more water absorbing agents. Suitable water-absorbing agents and/or absorbent materials comprising water-absorbing agents according to the invention are detailed below.

hydrogel forming absorbent polymers

The absorbent polymers of the present invention preferably comprise at least one hydrogel-forming absorbent polymer (also called hydrogel-forming polymer). Hydrogel-forming polymers useful in the present invention include a variety of water-insoluble but water-swellable polymers that are capable of absorbing aqueous liquids. Such hydrogel-forming polymers are well known in the art, any of which may be used in the present invention.

Hydrogel-forming absorbent polymers, also commonly referred to as "hydrocolloids" or "absorbent" materials, can include polysaccharides such as carboxymethyl starch, carboxymethyl cellulose, and hydroxypropyl cellulose; nonionics, such as polyvinyl alcohol and Polyvinyl ethers; cationic types such as polyvinylpyridine, polyvinylmorpholine (morpholinione) and N,N-dimethylaminoethyl or N,N-diethylaminopropyl acrylate and methacrylate and other respective season salt. Typically, hydrogel-forming absorbent polymers useful in the present invention have a multiplicity of anionic or cationic functional groups, such as sulfonic acid or amides or amino groups, and more typically carboxyl groups. Examples of polymers suitable for use in the present invention include those derived from polymerizable, unsaturated acid-containing monomers. Examples of cationic polymers having cationic groups are made from base-containing monomers. Thus, these monomers include ethylenically unsaturated acids and anhydrides which contain at least one carbon-carbon ethylenic double bond. More specifically, these monomers may be selected from olefinically unsaturated carboxylic acids and anhydrides, olefinically unsaturated sulfonic acids, and mixtures thereof. As noted above, the nature of the hydrogel-forming absorbent polymer is not critical to the present invention; however, selection of an optimal polymeric material can enhance the performance of the present invention. Preferred properties of absorbent polymers useful in the present invention are described below. These properties should not be construed as limiting; rather, they merely illustrate the progress that has been made in the field of absorbent polymers over the past few years.

In preparing the hydrogel-forming absorbent polymers of the present invention, some non-acid monomers, usually in minor amounts, may also be included. These non-acid monomers may include, for example, acid-containing monomers and water-soluble or water-dispersible esters that are completely free of carboxylic or sulfonic acid groups. Thus, optional non-acid monomers may include monomers containing functional groups of the following types: carboxylic acid or sulfonate, hydroxyl, amide, amino, nitrile, quaternary ammonium salt groups, aryl (e.g., phenyl such as those derived from styrene monomers). These non-acid monomers are known materials and are described in more detail in, for example, U.S. Patent 4,076,663 (Masuda et al.), issued February 28, 1978, U.S. Patent 4,062,817 (Westerman), issued December 13, 1977, Both documents are incorporated herein by reference.

Olefinated unsaturated carboxylic acid and carboxylic acid anhydride monomers include acrylic acid, typically acrylic acid itself, methacrylic acid, ethacrylic acid, alpha-chloroacrylic acid, alpha-cyanoacrylic acid, beta-methacrylic acid (crotonic acid), α-phenylacrylic acid, β-acryloxypropionic acid, sorbic acid, α-chlorosorbic acid, angelic acid, cinnamic acid, p-chlorocinnamic acid, β-steroidal acrylic acid, itaconic acid, citric acid Citronolic acid, mesaconic acid, glutaconic acid, aconitic acid, maleic acid, fumaric acid, vinyl tricarboxylate, and maleic anhydride.

Olefinated unsaturated sulfonic acid monomers include aliphatic or aromatic vinyl sulfonic acids such as vinyl sulfonic acid, allyl sulfonic acid, vinyl toluene sulfonic acid and styrene sulfonic acid; acrylic and methacrylic sulfonic acids such as acrylic sulfonic acid Ethyl ester, sulfoethyl methacrylate, sulfopropyl acrylate, sulfopropyl methacrylate, 2-hydroxy-3-methacryloxypropyl sulfonic acid and 2-acrylamide-2-methylpropyl sulfonic acid acid.

Preferred hydrogel-forming absorbent polymers useful in the present invention contain carboxyl groups. These polymers include hydrolyzed starch-acrylonitrile graft copolymers, partially neutralized hydrolyzed starch-acrylonitrile graft copolymers, starch-acrylic acid graft copolymers, partially neutralized starch-acrylic acid graft copolymers, saponified Vinyl acetate-acrylate copolymers, hydrolyzed acrylonitrile or acrylamide copolymers, microreticular cross-linked polymers of any of the above copolymers, partially neutralized polyacrylic acid and microreticular networks of partially neutralized polyacrylic acid cross-linked polymers. These polymers may be used alone or in the form of a mixture of two or more different polymers. Examples of these polymeric materials are disclosed in US Patent 3,661,875, US Patent 4,076,663, US Patent 4,093,776, US Patent 4,666,983, and US Patent 4,734,478.

The most preferred polymeric materials useful in the preparation of hydrogel-forming absorbent polymers are slightly network crosslinked polymers of partially neutralized polyacrylic acid and its starch derivatives. Most preferably, the hydrogel-forming absorbent polymer comprises from about 50% to about 95%, preferably about 75%, of neutralized, slightly network crosslinked polyacrylic acid (ie, poly(sodium acrylate/acrylic acid)). Network crosslinking renders the polymer substantially water insoluble, which in part determines the absorbent capacity of the hydrogel-forming absorbent polymer and the nature of the extractable polymer species. Methods of network crosslinking these polymers and typical network crosslinking agents are described in more detail in US Patent 4,076,663.

Although the hydrogel-forming absorbent polymers are preferably of one type (ie, homogeneous), mixtures of polymers may also be used in the present invention. For example, mixtures of starch-acrylic acid graft copolymers and slightly network crosslinked polymers of partially neutralized polyacrylic acid are useful in the present invention.

The hydrogel-forming polymer component may also be in the form of a mixed bed ion exchange composition comprising a cation-exchange hydrogel-forming absorbent polymer and an anion-exchange hydrogel-forming absorbent polymer. These mixed bed ion exchange compositions are described, for example, in U.S. Patent Application 09/130,321 filed January 7, 1998 by Ashraf et al. APPLIED PRESSURE"); and US Patent 6,121,509; the foregoing publications are incorporated herein by reference.

Hydrogel-forming absorbent polymers useful in the present invention can have a variety of sizes, shapes and/or morphologies. These polymers can be particulate, the ratio of the largest dimension to the smallest dimension is not very large (e.g., granules, powders, intergranular aggregates, intergranular cross-linked aggregates, etc.), fibers, sheets, films, foams, sheets and other forms. The hydrogel-forming absorbent polymers may also include minor amounts of one or more mixtures of additives, such as powdered silica, zeolites, activated carbon, molecular sieves, surfactants, gums, binders, and the like. The components in the mixture may be in a physically and/or chemically associated form such that the hydrogel-forming polymer component and the non-hydrogel-forming polymer additive do not readily separate physically.

Hydrogel-forming absorbent polymers are substantially non-porous (ie, have no internal porosity), or have substantial internal porosity.

For the above particles, particle size refers to the size determined by sieve size analysis. Thus, for example, particles retained on a U.S. Standard Test sieve with 710 micron openings (e.g., U.S. Series Spacer Sieve Designation No. 25) are considered to have a size greater than 710 microns; Particles on a sieve with 500 micron openings (eg, US Series Spacer Sieve Designation No. 35) are considered to have a particle size between 500 and 710 μm; particles that pass through a sieve with 500 micron openings are considered to have a particle size less than 500 μm. The mass-average particle size of a given sample of hydrogel-forming absorbent polymer particles is the particle size that divides the sample in half on a mass basis, i.e., half the sample by weight has a particle size smaller than the mass-average size and half the sample has The particle size is larger than the mass average size. When the 50% mass value does not correspond to the size aperture of an American Standard Test sieve, the standard particle size plot method (in which the cumulative weight percent of a sample of particles retained or passed through a given sieve size aperture on graph paper relative to the Sub-size pore plotting) is typically used to determine the mass average particle size. These methods of measuring particle size of hydrogel-forming absorbent polymer particles are further described in US Patent 5,061,259 (Goldman et al.), issued October 29, 1991, which is incorporated herein by reference.

For particles of hydrogel-forming absorbent polymers useful in the present invention, the particles typically have a particle size of from about 1 to about 2000 microns, more preferably from about 20 to about 1000 microns. The mass average particle diameter is generally about 20 to about 1500 μm, more preferably about 50 μm to about 1000 μm, even more preferably about 100 to about 800 μm. For embodiments comprising films, membranes, foams, fibers or polymers coated on a substrate such as a nonwoven, particle sizes larger than those described above are also suitable, or even preferred.

In particular embodiments, other properties of the absorbent polymer are also relevant. In these embodiments, the material may have one or more properties described in U.S. Patent No. 5,562,646 issued to Goldman et al. on October 8, 1996 and U.S. Patent No. 5,562,646 issued to Goldman et al. 5,599,335, each of which is incorporated herein by reference.

The basic hydrogel-forming absorbent polymers can be prepared in any conventional manner. Typical preferred methods of preparing these polymers are described in U.S. Reissued Patent 32,649 (Brandt et al.), issued April 19, 1988, U.S. Patent 4,666,983 (Tsubakimoto et al.), issued May 19, 1987, US Patent 4,625,001 (Tsubakimoto et al.), issued November 25, all of which are incorporated herein by reference.

Preferred methods for forming basic hydrogel-forming absorbent polymers are those involving aqueous or other solution polymerization. Aqueous solution polymerization involves the use of an aqueous reaction mixture to carry out the polymerization reaction, as described in the above-cited US Reissued Patent 32,649. The aqueous reaction mixture is then subjected to polymerization conditions sufficient to produce a substantially water-insoluble, slightly network crosslinked polymer in the mixture. The resulting mass of polymer can then be ground or chopped to form individual particles.

More specifically, the aqueous polymerization process for preparing hydrogel-forming absorbent polymers involves preparing an aqueous reaction mixture in which to carry out the polymerization. One component of such a reaction mixture is a monomer containing acidic groups which can form the "backbone" of the hydrogel-forming absorbent polymer to be prepared. The reaction mixture typically includes about 100 parts by weight of monomer. Another component of the aqueous reaction mixture includes a network crosslinker. Network crosslinking agents useful in forming the hydrogel-forming absorbent polymers of the present invention are described in more detail in the above-referenced US Reissued Patent 32,649, US Patent 4,666,983, and US Patent 4,625,001. The crosslinking agent is generally present in the aqueous reaction mixture in an amount of from about 0.001 mole percent to about 5 mole percent (about 0.01 to about 20 share). Optional components of the aqueous reaction mixture include free radical initiators including, for example, peroxy compounds such as sodium, persulfuric and ammonium persulfates, octanoyl peroxide, benzoyl peroxide, hydrogen peroxide, Cumene hydroperoxide, tert-butyl diperphthalate, tert-butyl perbenzoate, sodium peracetate, sodium percarbonate, etc. Other optional components of the aqueous reaction mixture include various non-acidic comonomers, including substantially unsaturated monomers containing acidic functionality or other comonomers that do not contain carboxylic or sulfonic acid functionality.

The aqueous reaction mixture is subjected to polymerization conditions sufficient to produce a substantially water-insoluble, but water-swellable, hydrogel-forming, absorbent, slightly network-crosslinked polymer in the mixture. The polymerization conditions are also discussed in more detail in the above three patent documents. These polymerization conditions generally include heating (thermal activation technique) to a polymerization temperature of from about 0°C to about 100°C, more preferably from about 5°C to about 40°C. Maintaining the polymerization conditions of the aqueous reaction mixture also includes, for example, subjecting the reaction mixture or a portion thereof to any conventional form of polymerization activating radiation. Radiation, electrons, ultraviolet and electromagnetic radiation are also alternative conventional polymerization techniques.

The acidic functional groups of the hydrogel-forming absorbent polymers in the aqueous reaction mixture are also preferably neutralized. Neutralization can also be carried out in any conventional manner such that at least about 25 mole percent, more preferably at least about 50 mole percent, of the total monomers used to form the polymer are acid group-containing monomers that are formed into Salt cation neutralization. These salt-forming cations include, for example, alkali metal, ammonium, substituted ammonium, and amines, which are discussed in more detail in above-referenced US Reissued Patent 32,649.

While it is preferred to prepare the particulate hydrogel-forming absorbent polymers using aqueous polymerization methods, it is also possible to practice using polymerization methods using heterogeneous polymerization processing techniques such as inverse emulsion polymerization or inverse suspension polymerization methods. In the inverse emulsion polymerisation or inverse suspension polymerisation process, the aforementioned aqueous reaction mixture is suspended in the form of tiny droplets in a matrix of a water-immiscible, inert organic solvent such as cyclohexane. The resulting particles of hydrogel-forming absorbent polymer are generally spherical in shape. The inverse suspension polymerization process is described in more detail in US Patent 4,340,706 (Obaysashi et al.), issued July 20, 1982, US Patent 4,506,052 (Flesher et al.), issued March 19, 1985, and April 5, 1988. US Patent 4,735,987 (Morita et al.), all of which are incorporated herein by reference.

Surface crosslinking of the initially formed polymer is a preferred method of obtaining hydrogel-forming absorbent polymers with properties including a relatively high porosity hydrogel layer ("PHL"), performance under pressure, ("PUP"), capacity and saline flow conductivity ("SFC") values, which are advantageous in the context of the present invention. Generally suitable methods of surface crosslinking the hydrogel-forming absorbent polymers of the present invention are disclosed in U.S. Patent 4,541,871 (Obayashi), published September 17, 1985; PCT Application WO 92/16565, published October 1, 1992 ( Stanley), PCT application WO90/08789 (Tai), published August 9, 1990; PCT application WO93/05080 (Stanley), published March 18, 1993; U.S. Patent 4,824,901 (Alexander ); U.S. Patent 4,789,861 (Johnson), issued January 17, 1989; U.S. Patent 4,587,308 (Makita), issued May 6, 1986; U.S. Patent 5,164,459 (Kimura et al.), published on August 17; German Patent Application 4,020,780 (Dahmen), published on August 29, 1991; European Patent Application 509,708 (Gartner), published on October 21, 1992; all of which are This article is incorporated by reference. See also US Patent 5,562,646 (Goldman et al.), issued October 8, 1996, and US Patent 5,599,335 (Goldman et al.), issued February 4, 1997, both of which are incorporated herein by reference.

For some embodiments of the present invention, it is advantageous if the hydrogel-forming absorbent polymer particles prepared in accordance with the present invention are typically substantially dry. As used herein, the term "substantially dry" refers to particles having a liquid content, typically water or other solution, of less than about 50%, preferably less than about 20%, more preferably less than about 10%, by weight of the particle. Typically, the liquid content of the particles of hydrogel-forming absorbent polymers ranges from about 0.01% to about 5% by weight of the particles. Individual particles can be dried by any conventional method, such as heating. Alternatively, when an aqueous reaction mixture is used to prepare the particles, water can be removed from the reaction mixture by azeotropic distillation. The aqueous reaction mixture containing the polymer can also be treated with a dehydrating solvent such as methanol. Combinations of these drying methods can also be used. The dehydrated polymer mass can then be chopped or ground to form particles of the substantially dry hydrogel-forming absorbent polymer.

Other gelling polymers

Acrylamide based gels are also suitable for use in the present invention. Specifically suitable are acrylamido, 2-(acryloyloxy)ethyl phosphate, 2-acrylamido-2-methylpropanesulfonic acid, 2-dimethylaminoethylacrylate, 2,2 '-bis(acrylamido) acetic acid, 3-(methacrylamido) propyl trimethyl ammonium chloride, acrylamido methyl propane dimethyl ammonium chloride, acrylate, acrylonitrile, acrylic acid, di Allyl dimethyl ammonium ammonium chloride, diallyl ammonium chloride, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, ethylene glycol, dimethacrylate, ethyl Diol monomethacrylate, methacrylamide, methacrylamidopropyltrimethylammonium chloride, N,N-dimethylacrylamide, N-[2[[5-(dimethyl Amino)1-naphthyl]sulfo]amino[ethyl1-2-acrylamide, N-[3-dimethylamino)propyl]acrylamide hydrochloride, N-[3-(dimethylamino )propyl)methacrylamide hydrochloride, poly(diallyldimethylammonium chloride), 2-(2-carboxybenzoyloxy)ethyl sodium methacrylate, sodium acrylate, alkene Sodium Propyl Acetate, Sodium Methacrylate, Sodium Styrene Sulfonate, Sodium Vinyl Acetate, Triallylamine, Trimethyl(N-Acryloyl-3-Aminopropyl) Ammonium Chloride, Triphenylmethane- Colorless parent derivatives, vinyl-terminated polymethylsiloxane, N-(2-ethoxyethyl)acrylamide, N-3-(methoxypropyl)acrylamide, N-(3- Ethoxypropyl)acrylamide, N-cyclopropylacrylamide, N-n-propylacrylamide and N-(tetrahydrofuryl)acrylamide.

Also suitable are gels based on N-isopropylacrylamide. These may include N-isopropylacrylamide, 2-(diethylamino)ethyl methacrylate, 2-(dimethylamino)ethyl methacrylate, 2-acrylamido-2-methyl -1-propane sulfoacrylate, acrylic acid, acrylamide,

Alkyl methacrylate, bis(4-dimethylamino)phenyl)(4-vinylphenyl)methyl leucocyanide, concanavalin A (lecithin), hexyl methacrylate, Lauryl Methacrylate, Methacrylic Acid, Methacrylamidopropyltrimethylammonium Chloride, n-Butyl Methacrylate, Poly(tetrafluoroethylene), Polytetramethylene Ether Glycol, Sodium Acrylate , sodium methacrylate, sodium vinylsulfonate, and vinyl-terminated polymethicone.

Also suitable are gels based on N,N'-diethylacrylamide. These may include N,N'-diethylacrylamide, methacrylamidopropyltrimethylammonium chloride, N-acryloyloxysuccinimide ester, N-tert-butylacrylamide and Sodium methacrylate.

Acrylate based gels are also suitable. These may include 2-dimethylaminoethyl acrylate, 2-acrylamido-2-methylpropanesulfonic acid, acrylamide, triallylamine, acrylate, acrylamide, methyl methacrylate , divinylbenzene, N,N-dimethylaminoethyl methacrylate, poly(oxytetramethylene dimethacrylate), poly(2-hydroxyethyl methacrylate), poly(2-hydroxypropyl methacrylate) and polyethylene glycol methacrylate.

Also suitable are gels based on various monomers. These may include acrylic acid, methacrylamidopropyltrimethylammonium chloride, collagen, dipalmitylphosphatidylethanolamine, poly[4-6-decadiene-1,10-diol bis(n-butoxycarbonylmethyl urethane)], poly[bis[aminoethoxy)ethoxy]phosphazene], poly[bis[(butoxyethoxy)ethoxy]phosphazene], poly[bis[ethyl oxyethoxy)ethoxy]phosphonazine], poly[bis[methoxyethoxyethoxy]phosphonazine], poly[bis[methoxyethoxy)phosphonazine], polydi Methylsiloxane, polyethylene oxide, poly(ethylene-dimethylsiloxane-ethylene oxide), poly(N-acryloylpyrrolidine), poly[n,n-dimethyl-N -[(methacryloyloxyethyl]-N-(3-sulfopropyl)ammonium betaine], polymethacrylic acid, polymethacryloyl dipeptide, polyvinyl alcohol, polyvinyl alcohol-vinyl acetate, Polyvinyl methyl ether, furan-modified poly(n-acetylethyleneimine), and maleimide-modified poly(n-acetylethyleneimine).

Also suitable as hydrogels are hydrogels comprising monomers selected from the group consisting of hydroxyalkylacrylates, hydroxyalkylmethacrylates, N-substituted acrylamides, N-substituted isoacrylamides, N-vinyl-2-pyrrolidone, N-acryloylpyrrolidone, acrylic acid, methacrylic acid, vinyl acetate, acrylonitrile, styrene, acrylic acid, methacrylic acid, crotonic acid, sodium styrenesulfonate, 2-sulfonic acid Sodium acyloxyethyl methacrylate, 2-acrylamido-2-methylpropanesulfonic acid, vinylpyridine, aminoethyl methacrylate, 2-methacryloyloxytrimethylammonium chloride, N , N'-methylenebisacrylamide, poly(vinyl alcohol) dimethacrylate, 2,2'-(o-phenylenedioxydiethyl dimethacrylate, divinylbenzene and triene Propylamine.

Also suitable gels are disclosed in US Patent 4,555,344, US Patent 4,828,710, and European Patent Application 648,521 A2 (both of which are incorporated herein by reference).

high surface area substances

In addition to osmotic absorbents (eg, hydrogel-forming absorbent polymers), the present invention may also include high surface area materials. It is this high surface area material which, alone or in combination with hydrogel-forming absorbent polymers, provides the separation apparatus or container with high capillary adsorption absorbent capacity. As discussed herein, high surface area materials are described in one aspect in terms of their absorbent capacity for capillary adsorption (measured in a separation apparatus or vessel that does not contain a hydrogel-forming polymer or any other optional material). It is recognized that substances with a high surface area can have an uptake capacity of very high suction heights (eg, 100 cm or higher). This allows high surface area materials to provide one or both of: i) liquid capillary pathways for osmotic absorbents; and/or ii) additional absorbent capacity. Therefore, although high surface area substances may be described in terms of their surface area per weight or volume, applicants of the present invention additionally use the absorbent capacity of capillary adsorption to describe high surface area substances, because the absorbent capacity of capillary adsorption is a performance parameter, which is generally given to the present invention. The separation device or container used by the invention provides the required intake capacity, resulting in an improved absorbent article. It will be appreciated that certain high surface area materials such as glass microfibers do not by themselves have particularly high capillary adsorption capacity at all heights, especially at very high heights (eg 100 cm or higher). However, these substances can provide the desired capillary pathway for liquid to hydrogel-forming absorbent polymers or other osmotic absorbents, thereby providing the desired absorbent capacity for capillary adsorption when they are combined with hydrogel-forming polymers or other osmotic absorbents. When absorbers are combined, this is possible even at very high altitudes.

Any material having sufficient absorbent capacity for capillary adsorption may be used in the separation apparatus or container of the present invention when used with hydrogel-forming absorbent polymers or other osmotic absorbents. In this context, the term "high surface area material" refers to any material that inherently has an absorbent capacity for one or more of the following capillary adsorption (i.e., in the absence of osmotic absorbent or any other optional material in the separation apparatus or vessel measured value): (1) at a suction height of 100 cm, the absorption capacity of capillary adsorption is at least about 2 g/g, preferably at least about 3 g/g, still more preferably at least about 4 g/g, still more preferably at least about 6 g/g (II) at a height of 35 cm, the absorbent capacity of capillary adsorption is at least about 5 g/g, preferably at least about 8 g/g, more preferably at least about 12 g/g; (III) at a height of 50 cm, the absorbent capacity of capillary adsorption is At least about 4 g/g, preferably at least about 7 g/g, more preferably at least about 9 g/g; (IV) at a height of 140 cm, the absorption capacity of capillary adsorption is at least about 1 g/g, preferably at least about 2 g/g, more preferably at least about 3 g/g, still more preferably at least about 5 g/g; or (v) at a height of 200 cm, the absorption capacity of capillary adsorption is at least about 1 g/g, preferably at least about 2 g/g, more preferably at least about 3 g/g , Still more preferably at least about 5 g/g.

In one embodiment, the high surface area material is of fibrous nature (hereinafter "high surface area fibers") to provide a fibrous web or matrix of fibers when combined with a hydrogel-forming absorbent polymer or other osmotic absorbent. Alternatively, the high surface area material is an open cell, hydrophilic polymeric foam (hereinafter "high surface area polymeric foam" or more generally "polymeric foam"). These substances are described in detail below.

High surface area fibers useful in the present invention include those natural (modified or unmodified) as well as synthetic fibers. High surface area fibers have a surface area much greater than the surface area of fibers typically used in absorbent articles such as wood pulp fibers. The high surface area fibers used in the present invention are desirably hydrophilic. As used herein, the term "hydrophilic" means that fibers or fiber surfaces are wettable by aqueous liquids (eg, aqueous body fluids) deposited on these fibers. Hydrophilicity and wettability are typically defined in terms of the contact angles and surface tensions of the liquids and solids involved. This is discussed in detail in "Contact Angle, Wettability and Adhesion", edited by Robert F. Gould, published by the American Chemical Society, (Copyright 1964). It is said that when the contact angle between the liquid and the fiber or its surface is less than 90 degrees, or when the liquid tends to spread spontaneously along the surface of the fiber, these two conditions usually exist simultaneously, then the fiber or the surface of the fiber will be wetted by the liquid Wet (ie, hydrophilic). Conversely, if the contact angle is greater than 90 degrees and the liquid does not spontaneously spread along the surface of the fiber, then the fiber or its surface is considered to be hydrophobic. The hydrophilicity of the fibers useful in the present invention may be inherent in the fibers, or the fibers may be naturally hydrophobic fibers which have been treated to render them hydrophilic. Materials and methods for imparting hydrophilicity to naturally hydrophobic fibers are known.

The high surface area fibers useful in the present invention have capillary suction specific surface areas in the same range as the polymeric foams described below. Typically, however, high surface area fibers are characterized by a BET surface area.

High surface area fibers useful in the present invention include glass microfibers such as those available from Evanite Fiber Corp. (Corvallis, OR). Typical fiber diameters of glass microfibers useful in the present invention are no greater than about 0.8 μm, more typically about 0.1 μm to about 0.7 μm. These microfibers have a surface area of at least about 2 m ² /g, preferably at least about 3 m ² /g. Typically, the glass microfibers have a surface area of from about 2 m ² /g to about 15 m ² /g. Representative glass microfibers useful in the present invention are those commercially available from Evanite Fiber Corp. as Type 104 glass fibers having a nominal fiber diameter of about 0.5 μm. The calculated surface area of these glass microfibers is about 3.1 m ² /g.

Another class of high surface area fibers useful in the present invention are fibrillated cellulose acetate fibers. These fibers (referred to herein as "fibret") have a high surface area relative to fibers derived from cellulose, which are commonly used in the field of absorbent articles. These fibers have very small diameter domains such that their grain width is typically from about 0.5 to about 5 μm. These fibers typically have a surface area of about 20 m ² /g. Representative fibers commonly used as high surface area materials in the present invention are commercially available from Hoechst Celanese Corp. (Charlotte, NC) under the tradename cellulose acetate Fiberts ^(R) . For a detailed discussion of fibers, including their physical properties and methods of preparation, see "CelluloseAcetate Fiberts: A Fibrillated Pulp With High Surface Area", Smith, JE, Tappi Journal, Dec.1988, p.237; and published in 1996 US Patent 5,486,410 (Groeger et al.), Jan. 23; each of the above publications is incorporated herein by reference.

In addition to these fibers, those skilled in the art will recognize that other fibers well known in the absorbent art can be modified to provide high surface area fibers for use in the present invention. Representative fibers that can be modified to achieve the high surface area required by the present invention are disclosed in the aforementioned US Patent No. 5,599,335 (see columns 21-24 in particular), which is incorporated herein by reference.

Regardless of the nature of the high surface area fibers used, the fibers and osmotic absorbent are dispersed substances prior to mixing. As used herein, the term "dispersed" means that the high surface area fibers and permeable absorbent are prepared separately prior to mixing to form the core of a separate device or vessel. In other words, the high surface area fibers are not made after mixing with an osmotic absorbent (eg, a hydrogel-forming absorbent polymer), nor is the osmotic absorbent made after mixing with the high surface area fibers. The mixing of the individual dispersed components ensures that the high surface area fibers will have the desired morphology and more importantly the desired surface area.

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Barrier materials can be used in the absorbent material of the present invention. Barrier materials suitable for use in the present invention include any fibrous or particulate material that is at most only slightly soluble in water and/or lipophilic fluids. The barrier material can be dispersed through the matrix of absorbent material to improve permeability above that of a matrix made of absorbent material alone; alternatively, the barrier material can be used to maintain permeability even after the absorbent material encounters water Permeability is maintained even after swelling and/or gelling. Thus, the barrier material helps to reduce the pressure drop across the matrix of absorbent material when fluid containing water passes through the matrix. In addition, if the absorbent material is prone to condensation after encountering water and subsequent collapse, the barrier material helps to reduce or prevent post-collapse gel freezing.

Non-limiting examples of suitable barrier materials include sand, silica, aluminosilicates, glass microspheres, clays, layered silicates, wood, natural textile materials, synthetic textile materials, alumina, alumina , aluminum silicate, zinc oxide, molecular sieve, zeolite, activated carbon, diatomaceous earth, silica hydrate, mica, microcrystalline cellulose, montmorillonite, peach pit powder, pecan shell powder, talc, tin dioxide , titanium dioxide, walnut shell powder, and particles of different metals or metal alloys. Also useful are particles made of mixed polymers (e.g., copolymers, terpolymers, etc.), such as polyethylene/polypropylene copolymers, polyethylene/propylene/isobutylene copolymers, polyethylene/propylene/isobutylene copolymers, etc. Styrene and its polymers, etc.

Other particulate materials useful in the present invention are synthetic polymer particles selected from polybutene, polyethylene, polyisobutylene, polymethylstyrene, polypropylene, polystyrene, polyurethane, nylon, Teflon, and their mixture. Of these, polyethylene and polypropylene particles are most preferred, and oxides of these substances are especially preferred. Examples of commercially available particles useful in the present invention include ACumist ^™ Micronized Polyethylene Wax available from AlliedSignal (Morristown, NJ) in series A, B, C and D in various average particle sizes of 5 microns to 60 microns. Preferred are ACumist ^™ A-25, A-30 and A-45 oxidized polyethylene particles having mean particle sizes of 25, 30 and 45 microns, respectively. Examples of commercially available polypropylene particles include the Propyltex series, available from Micro Powders (Dartek) and ACuscrub ^™ 51, available from Allied Signal (Morristown, NJ), which have an average particle size of about 125 microns.

absorption matrix

In order to increase the permeability of a "dry" absorbent matrix or to maintain its permeability when the absorbent matrix is wet, it is important to provide the barrier material with sufficient absorbent material and optionally a high surface area to substance ratio. Because the weight of the potential barrier material can vary widely depending on the weight of the absorbent material, this ratio must be quantified on a "dry" volume basis. "Net matrix volume" means the volume of absorbent material, barrier material, and optionally any high surface area material, which does not include any internal material volume that the material itself may contain or any volume for internal material void space. "Internal material void volume" refers to the total volume of voids between particles and/or fibers of a material, which voids typically arise naturally when the particles and/or fibers occupy a given space. "Dry bulk matrix volume" is equal to the net matrix volume combined with internal material voids at the base. For the present invention, it is preferred that the absorbent material comprises from 50% to 100%, more preferably from 75% to 95%, of the volume of the dry bulk matrix. Preferably, the insulating material comprises from 1% to 50%, more preferably from 5% to 25%, of the volume of the dry bulk matrix. Preferably, the optional high surface area material comprises from 1% to 50%, more preferably from 5% to 25%, of the volume of the dry bulk matrix.

The gel mass, barrier material and optional high surface area mass can be produced as woven or nonwoven fibrous structures, such as sheets or films or membranes, and shaped in different ways. Sheet configurations are application dependent and typically include four general configurations, namely tubes, hollow fibers, plate and frame elements, and helically wound modules, all of which are within the scope of the present invention.

The packing density of the water-absorbing agent on the fibrous structures of the present invention ranges from about 50 g of water-absorbing agent per square meter of fibrous structure to about 2000 g of water-absorbing agent per square meter of fibrous structure.

A tube is perhaps the simplest configuration in which a thin plate is cast on the inner wall of a porous support tube. However, the tube configuration is not cost feasible since the porous support tube itself is the major cost factor.

In theory, hollow fibers are the ideal thin-plate configuration because there is no "parasitic" drag and no expensive porous support tubes. These fibers can be pressurized internally, which can create "narrow channel" fluid control of aqueous fluids. However, the biggest disadvantage of hollow fibers is the pressure constraint, which limits the lateral flow velocity along the fiber duct. Additionally, the hollow fiber configuration is more prone to fouling and clogging than the other three configurations; however, larger diameter fibers are gaining popularity for improved fouling resistance. Fortunately, hollow fibers are easily cleaned by backwashing, which tends to compensate for their tendency to foul. Conversely, backwashing of tubes, plate and frame units, and spiral wound modules is not recommended due to problems with membrane delamination and glue seam seal failure.

Flat panels within panel and frame units offer the most versatility; they are also the most cost constrained.

Although spiral wound modules were originally developed for reverse osmosis, they are increasingly gaining share in the UF market by offering one of the cheapest UF modules in terms of cost per plate area unit. Spiral wound units cannot be unwound for cleaning, and most spiral wound units cannot be autoclaved. They fall somewhere between hollow fiber and tubes (and more expensive plate and frame units) in terms of tendency to get dirty.

Gel materials can also be deposited directly onto fibrous structures or insulating materials. This can be achieved by first applying an aqueous monomer solution containing 10% to 100% water soluble unsaturated monomer to the fibrous structure or insulation material and then polymerizing the monomer.

The thickness of the fibrous structure generally ranges from 0.01 to 10 mm, preferably from 0.1 to 5 mm. The basis weight of the nonwoven fabric is desirably in the range of 5 to 1000 g/square meter, preferably 10 to 300 g/square meter.

The method of the invention

The present invention can optionally be combined with several well-known methods to purify fluids. These methods can be used to assist in the separation operation of the water-lipophilic fluid and/or to remove impurities from the lipophilic fluid after it has been used.

Distillation is the process of producing vapors by heating a liquid in a container, then condensing the vapors and collecting them in another container. Available distillation methods are simple distillation, fractionation, steam distillation, immiscible solvents, azeotropic distillation, extraction, vacuum distillation, molecular distillation, entrainer sublimation, and freeze-drying.

Extraction is the selective transfer of compounds from one liquid to another immiscible liquid or from a solid to a liquid. The former method is called liquid-liquid extraction, which is an indirect separation technique because the two components are not directly separated. Foreign matter, immiscible liquids are introduced to provide the second phase.

"Decanting" and "density fractionation" are gravity-type separation methods. A "decanter" is defined as a vessel used to continuously separate a stream into two liquid phases by gravity. Using Stokes' law, the settling rate of small droplets in the continuous phase can be derived and the decanter can be designed accordingly.

Ion exchange is the process by which one ion in a compound is exchanged for a different ion of the same type: a cation is exchanged for another cation, and an anion is exchanged for another anion. Ion exchange resins are typically used to perform the exchange. All ion exchange resins, whether they are cation or anion exchangers, strongly or weakly ionizing, gel or macroporous, spherical or granular, can be considered as solid solutions. In fact, any observed ion exchange behavior can be rationalized on the basis of the component partitioning of the two solution phases, one of which is confined to the solid phase. The transfer of components occurs through the phase interface, which is the surface of the bead or particle. The internal phase of ion exchange resins contains four essential components. The components include: a three-dimensional polymer network, ionic functional groups permanently bound to the network, counterions, and solvents. Under certain conditions, there may be other components in the resin, such as secondary solvents, co-ionic and non-ionic solutions.

Adsorption, such as by activated carbon, is an important unit operation for separating liquids and exploits surface phenomena that occur on the surface of absorbent materials. Adsorption occurs when the energy associated with the solid surface attracts molecular or ionic species from the liquid to the solid. The adsorbed material can form a one to several molecule thick layer on the surface. The amount and nature of the surface as well as the environmental conditions on the surface will control adsorption. When in contact with a wet absorbent mixture, several highly porous solids preferentially adsorb and remove water to very low concentrations. Although they can be used on a disposable basis, they can be regenerated by heating. Molecular sieves are commonly used; however, organic adsorbents such as ion exchange resins are attractive alternatives.

Chromatography is a multistage separation technique based on differences between compounds adsorbed to surfaces or dissolved in thin films of liquids. The more common types of chromatography are paper, thin layer, high performance, gas phase, and gel permeation. The two main mechanisms at work during chromatographic separations are displacement and partition.

Dialysis is the transfer of solutes across membranes resulting from a transmembrane gradient of solute concentration. It is accompanied by osmosis, which is the transfer of solvent across the membrane due to a transmembrane gradient of solvent concentration. The direction of solute transfer in dialysis is opposite to that of solvent transfer in osmosis. Dialysis is effective in removing low molecular weight solute molecules or ions from solution by their passage through semipermeable membranes driven by a concentration gradient.

Electrodialysis is the transfer of electrolytes through solution systems and membranes under an electrical driving force. As presently used, the term electrodialysis refers to multi-compartment electrodialysis with ion exchange membranes. There are four variants of electrodialysis: electrolysis, concentration dilution, ion displacement, and reversal.

Diafiltration differs from conventional dialysis in that the removal rate of microspecies does not depend on concentration, but is a simple function of the ultrafiltration rate (membrane area) in relation to the volume to be exchanged or dialyzed. Repeated or sequential solvent additions can effectively and rapidly flush out or exchange salts and other microspecies.

Solids can be designed to adsorb water while rejecting solvents. Similarly, membranes can be designed to pass water and retain solvent or vice versa. The use of pervaporation for removal of water from solvent-water mixtures involves the use of hydrophilic membranes. Preferred membranes are polyvinylidene fluoride membranes such as Osmonic JX (trade name), polysulfone type hollow fiber membranes from AG, and silanized cellulose filters from Whatman. Solvent removal from water is exactly the same except that a membrane that rejects water is used but is lipophilic.

Crystallization is the process by which crystals are produced from vapor, melt, or solution, and is distinguished from precipitated phases in that the latter typically display high levels of supersaturation, primary nucleation, and low solubility ratios.

Centrifugation is a technique for separating substances based on density differences, the rate of separation being increased by the application of increasing rotational force. This force is called centrifugal force, and the device that provides the turning force is called a centrifuge.

Cassette filtration is primarily used to remove solids from liquids. Specifically, low solids liquids are filtered to render them visually clear solutions. Cassettes are available in cylindrical configuration, with pleated or unpleated, disposable or washable filter media. The filter media is usually integrally bonded to plastic or metal hardware.

Settling is the separation of suspended solid particles from a liquid stream by gravity settling. Sedimentation can also be used to separate solid particles based on differences in their sedimentation rates.

Stripping is a method of removing many of the organic solvents in wastewater to levels where the water can be discharged. This method is especially suitable for solvents with low solubility in water or high volatility associated with water.

Desiccant drying involves contacting a water-wet solvent with a solid, usually an electrolyte, suitable for absorbing water and forming a second phase. Water can then be removed from this second phase by other means such as decanting.

Chemical addition involves adding chemicals to change at least one physicochemical property of a liquid, such as pH, ionic strength, and the like. Examples of these chemicals include salts, acids, bases, coagulants and flocculants.

Addition of enzymes, microorganisms or bacteria involves adding enzymes, microorganisms or bacteria to a waste stream to remove organic contaminants from the stream.

Temperature regulation enhances the separation of binary mixtures and can include both cooling and/or heating of the mixture. Increasing the temperature of the mixture aids bonding, while cooling aids crystallization or solidification of one of the components.

Electrostatic binding involves exposing an emulsion comprising two immiscible phases (e.g. lipophilic fluid and water), one continuous and the other discontinuous, to an electric field, thereby affecting the binding of the discontinuous phases into a sufficiently large size such that the droplets fall from the emulsion based on the density difference of the two phases. In order to implement this method, the two phases must have at least slight differences in dielectric constant and density. Galvanic bonding is a well-known method described in US Patent 3,207,686 to Jarvis et al.; 3,342,720 to Turner; US Patent 3,772,180 to Prestridge; US Patent 3,939,395 to Prestridge; Patent 4,126,537; US Patent 4,308,127 to Prestridge and US Patent 5,861,089 to Gatti et al.

Absorption involves exposing the emulsion to a substance that absorbs at least one component from the emulsion. Absorbent materials typically undergo volume changes (or expansion or contraction), as opposed to adsorption, which is primarily a surface phenomenon. In one embodiment, absorbent polymers can be utilized to remove water from solvent-water emulsions.

method

The present invention relates to a method of treating a lipophilic fluid contained in an emulsion consisting at least of water and a lipophilic fluid. The method includes the steps of pretreating the emulsion, recovering the lipophilic fluid from the emulsion, and purifying the lipophilic fluid. The method may further comprise the step of first exposing the fabric to the lipophilic fluid and water, and then collecting the lipophilic fluid and water in the form of an emulsion. The method may optionally include a mixing step, wherein at least a portion of the lipophilic fluid and at least a portion of the water are mixed to form an emulsion prior to exposure to the fabric. Emulsifiers may also be added during the mixing step.

If emulsifiers are included at all, the emulsion may include about 10% by weight of emulsifiers. Preferably, the lipophilic fluid and aqueous emulsion have a water/lipophilic fluid/emulsion ratio of from about 1/98.9/0.1 to about 40/55/5 by weight of the emulsion. Finally, as discussed in the "Adjunct Ingredients" section, emulsifiers can also act as surfactants.

Preferably, lipophilic fluids include linear silicones, cyclic silicones and mixtures of these silicones. More preferably, these siloxanes are selected from octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane and mixtures of these siloxanes. Even more preferably the lipophilic fluid comprises decamethylcyclopentasiloxane. Finally, it is most preferred that the lipophilic fluid comprises decamethylcyclopentasiloxane and is substantially free of octamethylcyclotetrasiloxane.

The "collecting" step of the present invention can be implemented in several ways. Spinning fabric loads, including lipophilic fluids and water, is well known in conventional laundering applications. Twisting, twisting or squeezing the treated fabric is also a well known mechanical means of extracting fluids from fabrics and fabric articles. Evaporation can also be applied to collect lipophilic fluid and water and/or to dry the fabric load. Heating the fabric load, lipophilic fluid and water or other well known methods for evaporation can do this. Rotation and/or tumbling can be combined with heating to aid in evaporation and evaporation uniformity. If this method were used, subsequent condensation of the lipophilic fluid and water would be required, followed by recovery and purification steps.

The "pretreatment" step can be carried out by a variety of conventional methods. Non-limiting examples of pretreatment methods include sedimentation, centrifugation, exposure to rotational manipulation, decantation, filtration, chemical addition, and temperature adjustment. Pretreatment regimens may also include combinations of the foregoing methods.

If filtration is performed, it is desirable to pass the lipophilic fluid and aqueous emulsion through a filter of particulate matter such that particles or particle aggregates of about 25 microns or larger are removed, preferably such that particles of about 15 microns or larger or Particle aggregate removal, more preferably, such that particles or particle aggregates of about 10 microns or larger are removed, even more preferably, such that particles or particle aggregates of about 5 microns or larger are removed, even more preferably , such that particles or particle aggregates of about 1 micron or larger are removed. It is also possible to expose lipophilic fluids and aqueous emulsions to activated carbon for further pretreatment.

The "recovery" step can similarly be carried out by a variety of well known methods. Non-limiting examples of recovery methods include mechanical bonding, electrical bonding, chemical addition, membrane filtration, temperature regulation, steam stripping, microbial addition, exposure to absorbent material, centrifugation, distillation, adsorption, absorption, crystallization, precipitation, temperature regulation, Filtration, electrolysis, extraction, pH adjustment and ionic strength adjustment. One of the many possible ways to perform adsorption is to expose the emulsion to activated carbon. Recovery schemes may also include combinations of the above methods.

The "purification" step can be carried out in a variety of ways. Non-limiting examples include membrane filtration, distillation, extraction, precipitation, enzyme addition, ion exchange, desiccant drying, chromatography, and adsorption. Purification protocols may also include combinations of the above methods.

The invention also relates to methods of purifying lipophilic fluids and lipophilic fluid vapors. The method includes the steps of collecting lipophilic fluid vapor and a first emulsion comprising water and lipophilic fluid. The lipophilic fluid vapor is then condensed to form condensed lipophilic fluid vapor. The condensed lipophilic fluid vapor combines with the first emulsion to form a second emulsion. The second emulsion can then be pretreated as described above. After pretreatment, lipophilic fluid and condensed lipophilic fluid vapor can be recovered from the second emulsion in the same manner as described above. After recovery from the emulsion, the lipophilic fluid and condensed lipophilic fluid vapor are purified as described above. As in the first embodiment, this method may also optionally include the step of first exposing the fabric to the lipophilic fluid and water, and then collecting the lipophilic fluid and water in the form of a first emulsion. The method may optionally include a mixing step, wherein at least a portion of the lipophilic fluid and at least a portion of the water are mixed to form a first emulsion prior to exposure to the fabric. Emulsifiers may also be added during the mixing step.

Any of the compositions or emulsions discussed above may further comprise adjunct ingredients selected from the "Adjunct Ingredients" section above including, but not limited to, enzymes, bleaches, surfactants, fabric softeners, fragrances, antimicrobials , antistatic agent, whitening agent, dye curing agent, dye rubbing inhibitor, anti-bleaching agent, wrinkle reducing agent, anti-wrinkle agent, soil release polymer, sunscreen, anti-fading agent, auxiliary agent, foaming agent, composition Odor control agents, composition colorants, pH buffering agents, water repellents, stain repellents, and mixtures of these adjuvants.

The method and system of the present invention can be used in service industries, such as dry cleaning services, diaper services, uniform cleaning services, or business operations such as self-service laundry, dry cleaning machines, linen services, which are hotels, restaurants, conference centers, airports, tourism, etc. Part of a boat, port facility, casino, or can be used in a home.

In addition to conventional methods such as aqueous washing, the method of the invention can also be carried out in plants which are retrofitted to existing plants and which are modified in some way in order to carry out the method of the invention and related methods.

The method of the present invention may also be practiced in a device that is not a modification of an existing device, but a device that has been specially constructed in some way to practice the present invention, or may be part of a lipophilic fluid treatment system join another device. This will include all associated plumbing such as connections for chemical and water supplies and drainage for waste wash fluid.

The system of the present invention can be used in a plant that is not a modification of an existing plant, but a plant specially built in some way to practice the present invention and, possibly, conventional methods such as aqueous washing.

The method of the present invention may also be implemented in devices with "dual mode" functionality. A "dual mode" unit is one that is capable of washing and drying fabrics in the same drum. These devices are widely available, especially in Europe.

Apparatus for practicing the invention typically include some type of control system. These control systems include electrical systems, such as so-called intelligent control systems, as well as conventional electromechanical systems. The control system enables the user to select the volume of fabric load to be cleaned, the type of soil, the degree of soiling, and the timing of the cleaning cycle. Alternatively, the user may use pre-set cleaning and/or refresh cycles, or the device may control the cycle length based on any number of determinable parameters. This is especially true for electrical control systems. For example, when the collection rate of lipophilic fluid reaches a steady rate, the device can automatically shut off after a fixed period of time, or start another process of lipophilic fluid.

For electrical control systems, one option is to make the control devices so-called "smart devices". This means including, but not limited to, self-diagnostic systems, load type and cycle selection, connecting the machine to a network and allowing the consumer to remotely activate the unit, notifications when the unit has finished cleaning fabric items, or when the unit has malfunctioned Have the supplier remotely diagnose the problem. In addition, if the system of the present invention is only part of a cleaning system, so-called "smart systems" can be connected to other cleaning equipment, such as washing machines and dryers, which will be used to complete the remainder of the cleaning process.

Claims (14)

1. A method for processing said lipophilic fluid contained in an emulsion comprising water and a lipophilic fluid, said method comprising the steps of: a. pretreating the emulsion; b. recovering said lipophilic fluid from said emulsion; and c. Purifying the lipophilic fluid. 2. The method of claim 1, further comprising the steps of: a. exposing the fabric to said lipophilic fluid and said water; and b. collecting said lipophilic fluid and said water in said emulsion. 3. The method of claim 2, wherein said method also comprises a mixing step comprising mixing at least part of said lipophilic fluid with at least part of said water to form said emulsion prior to said exposure , preferably wherein an emulsifier is also added to said lipophilic fluid and said water during said mixing to form said emulsion. 4. The method of claim 2, wherein said collecting comprises rotating said fabric, said lipophilic fluid and said water. 5. The method of claim 2, wherein said collecting includes twisting said fabric. 6. The method of claim 2, wherein said collecting comprises evaporating at least a portion of said lipophilic fluid and at least a portion of said water, and condensing at least a portion of said lipophilic fluid and at least a portion of said water. 7. The method of claim 1, wherein the pretreatment is selected from the group consisting of sedimentation, centrifugation, exposure to rotational manipulation, decantation, filtration, temperature adjustment, chemical addition, and combinations thereof. 8. The method of claim 1, wherein said pretreatment comprises passing said emulsion through a filter to remove particles and particle aggregates of about 1 micron or larger. 9. The method of claim 1, wherein said recovering is selected from the group consisting of mechanical coalescence, electrical coalescence, chemical addition, membrane filtration, temperature regulation, steam stripping, microbial addition, exposure to absorbent material, centrifugation, distillation, adsorption , absorption, crystallization, precipitation, temperature adjustment, diafiltration, electrolysis, extraction, pH adjustment, ionic strength adjustment, and combinations thereof, preferably wherein said adsorption comprises exposing said emulsion to activated carbon. 10. The method of claim 1, wherein the purification is selected from the group consisting of membrane filtration, distillation, extraction, stripping, enzyme addition, ion exchange, desiccant drying, adsorption, and combinations thereof. 11. The method of claim 1, wherein the emulsion comprises up to about 10% emulsifier by weight of the emulsion, preferably wherein the emulsion comprises a ratio of about 1/98.9 by weight of the emulsion /0.1 to about 40/55/5 water/combined lipophilic fluid and condensed lipophilic fluid vapor/emulsifier, and/or wherein the emulsifier includes a surfactant. 12. The method of claim 1, wherein the lipophilic fluid comprises a linear siloxane, a cyclic siloxane, or a mixture thereof, preferably wherein the lipophilic fluid comprises a lipophilic fluid selected from the group consisting of : octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, and mixtures thereof, more preferably wherein said lipophilic fluid comprises decamethylcyclopentasiloxane even more preferably wherein the lipophilic fluid comprises decamethylcyclopentasiloxane and is substantially free of octamethylcyclotetrasiloxane. 13. The method of claim 1, wherein said emulsion also includes co-ingredients selected from the group consisting of enzymes, bleaches, surfactants, fabric softeners, fragrances, antibacterial agents, antistatic agents, whitening agents agent, dye curing agent, dye wear inhibitor, anti-bleaching agent, wrinkle reducing agent, anti-wrinkle agent, soil release polymer, sunscreen agent, anti-fading agent, adjuvant, foaming agent, composition odor control agent, composition coloring Agents, pH buffers, water repellents, stain repellents, and mixtures thereof. 14. The method of claim 10, wherein the membrane filtration comprises polyvinylidene fluoride membranes and/or polysulfone hollow fiber membranes and/or silanized cellulose membranes.