CS160291A3 - Agent and process for fireproof finish of fabrics and process to achieve fabrics burning retardation - Google Patents

Description

ma- for flame retardant fabric treatment

JUDr. Miloš VŠETEČKA * attorney / 2? o z f 'flfi 04 PRAHA 1, Zitna 25 - 1

Flame retardant fabric burning agent

Technical field

BACKGROUND OF THE INVENTION The present invention relates in particular to a composition for impregnating a fireproofing agent.

Background Art

Cotton fabrics can be treated to become flame retardant by impregnating them with various chemicals, thus providing a sustained or temporary fire resistance. Such chemistry includes antimony compounds, organic halogen compounds, and organic or inorganic phosphorus compounds, such as water-insoluble and soluble ammonium polyphosphates, which can be fixed in fabrics by heat (see, for example, GB-P-15045C7). In the processing of many fabrics, especially upholstery, it is important that the appearance and feel of the fabric is virtually unaffected by any flame retardant burning. Therefore, the upholstery fabrics adjust, to obtain the flame resistance of the back, in particular by using an antimony-containing resin composition and an organic bromine compound. These compositions are unnecessary environmental protection considerations and are moreover suitable only for low specific weight fabrics.

SUMMARY OF THE INVENTION

Now, a fabric retardant composition has been prepared for backing fabric that is suitable for a wide variety of fabric weights and more environmentally friendly. Accordingly, the present invention provides a flame retardant composition comprising (i) ammonium polyphosphate, at least partially water insoluble, (ii) a suds preventing agent, (iii) a thermosetting resin, and (iv) water, particularly preferably (v) ) a surfactant, (vi) a water-soluble polyphosphoric ammonium and / or (vii) carbamic acid derivative. The invention further relates to a method for achieving a flame retardancy of a fabric comprising impregnating the fabric with a composition comprising the aforementioned components (i) to (iv), and in particular also components (v), (vi) and / or (vii), this impregnated fabric cures with heat ·

v v

The invention also relates to a fabric which has not been burned by impregnating it with a composition comprising the aforementioned components (i) to (iv), and preferably also components (v), (vi) and / or (vii) where impregnated fabric, heat cured.

At least partially water-insoluble polyphosphate (referred to herein as insoluble) typically has a water solubility of less than 10 g in 100 g of water at 20 ° C, especially less than 8 or 5 g in 100 g of water, such as 0.1 g. up to 5, 0.5 to 3 or 1.5 to 7 g in 100 g of water, the solubility being determined by the test used by Manders Paint Company for ammonium polyphosphates used in coating compositions, as described below. This polyphosphate can be considered as a mixture of truly soluble and insoluble components, the soluble components of which can be leached by adding water or by introducing it into water, whereby an insoluble fraction with a high surface to volume ratio is obtained, e.g. very fine powder and / or honeycomb structure. It is possible to prepare by heating mono- or diammonium polyphosphate, either alone or mixed with phosphorus pentoxide or ammonia, at a temperature of, for example, 200 to 400 ° C. Phosphorus pentoxide can be charged, at least in part, with phosphoric acid and the source of ammonia can be urea (see, for example, British patents BP 1103772, 1184878, 1309873 and European patent EP 49763). Insoluble polyphosphate can have a straight or branched chain structure and the general formula (KH ^) and 2 ^ b®3b + 1 * wherein b has an average value greater than 10, a / b has a value in the range of 0.7 to 1.1 and a maximum of value a jeb + 2. The molecular weight of the insoluble polyphosphate is usually greater than 10,000, for example 10,000 to 2 million, such as 10,000 to 1,000,000 or 200,000 to 1,5 million. The water-insoluble ammonium polyphosphate typically has an average particle size of less than 50 microns, preferably less than 30 microns, such as 1 to 50, 5 to 50, or 10 to 30 microns; preferably at least 60% of the particles are less than 30 microns and especially at least 40% of the particles are finer than 10 microns. Typically, polyphosphate contains; 20 to 35% phosphorus, for example 23 to 32%, preferably 25 to 32% phosphorus. Examples of suitable insoluble polyphosphates are polyphosphates produced by Albright and Wilson Limited under the trade name AliGARD UC or AUGARD PI.

Typically, the composition according to the invention comprises (based on the weight of all components (i to vii)) 15 to 30%, for example 10 to 25% or 19 to 23% of water-insoluble ammonium polyphosphate, while based on the weight of the components (i to iv). ) comprises a composition of 15 to 30%, for example 20 to 28% or 21 to 25%, and in particular 24 to 27% of polyphosphate. The antifoaming agent is a substance that acts on a liquid that foams or is capable of foaming and contains a surfactant by reacting with the surfactant molecules and / or acting on the liquid / vapor interface to break the foam or prevent its formation. . Examples of such agents are soaps, alkyl esters of phosphoric acid and formulations based on mineral oil, wax, vegetable oil or silicone. Silicone-based formulations include liquid polysiloxanes which may be fluorosiloxanes or alkylsiloxanes optionally substituted with amino groups, and are preferably dimethylsiloxane polymers; they preferably also contain fine-dusted silica, which may be formed in situ by hydrolysis

Itetraalkoxysilanes. The preferred antifoam agent used in the composition of the present invention is manufactured by Wacker-ChemieGmbH under the designation S 132. 1 The composition according to the invention usually comprises 0.01 to 0.5%, e.g. preferably 0.05 to 0.2% of an antifouling agent foaming. | The thermosetting resin (iii) is derived from at least one ethylenically unsaturated monomer and may be a homopolymer; however, it is preferably a copolymer. Examples of suitable monomers are ethylene and monosubstituted ethylenes, for example vinyl esters of carboxylic acids, for example of 4 to 8 carbon atoms, such as vinyl ethers, ethylenes substituted by one or two carboxyl groups and their esters such as acrylic acid, methacrylic acid, maleic acid and esters thereof such as ethyl acrylate, and chloroethylenes such as vinyl chloride, and cyanoethylenes such as acrylonitrile. Preferred resins are copolymers comprising ε-δ-4 - 4 - acrylic monomer units alone or with acrylonitrile or vinyl chloride, or vinyl acetate / ethylene copolymers. Examples of suitable resins are those produced by Harlow Chemical Co., England under the name REVACRYL 274, or Vinamul Ltd, Surrey, England under the designation VINAMUL 3306, and BASF, Germany under the designationsLUTOFAN LA 560S and LUTOFAN 300d and ACRONAL DS 2272. -

The resin is usually sold in the form of an aqueous dispersion or emulsion, which usually contains an emulsifier, which may be anionic, such as some alkyl sulfate and / or alkyl ether sulfate, the mixture of which is present in the case of REVACRYL 274 resin, non-ionic, as in the case of a copolymer ethylene with vinyl acetate sold under the designation VINAMUL 3306. The dispersions typically contain 40 to 55% of the resin dry matter. Although the emulsifier added by the resin may suffice as the sole emulsifier for use in the compositions of the invention (as is the case with the acrylic copolymer with vinyl chloride sold under the name LUTOFAN 560S), a separate emulsifier may also be added. These resins typically have a temperature of Τθ less than 30 ° C, for example -40 to +30 ° C, and in particular 0 to 30 ° C. They are heat-curable by themselves, for example at 80 to 180 ° C, but especially at 120 to 170 ° C. The compositions of the invention typically contain 10 to 30% or 15 to 30%, for example 20 to 25%, 21 to 24% or 21.5 to 23.5% of the resin (expressed as the resin dry weight based on the total weight of the components (i to vii)), or 10 to 30%, for example 14 to 23%, such as 17 to 21% or 14 to 18% (based on the weight of the composition comprising components (i to v), but not (vi) or (vii)).

The compositions of the invention also contain, as component (iv), water in an amount of usually 40 to 51%, for example 42 to 50% or 44 to 49% (based on the weight of the components (i to vii), or 50 to 60%, e.g. 58% (based on the amount by weight of components (i to IV) in the absence of components (v), (vi) and (vii).

These numbers include water optionally added with other components, such as resin or surfactant, as well as water added separately.

The surfactant (component (v)) is usually a poor surfactant but with some surface activity. Preferably, it comprises a strong foaming agent, especially one which stabilizes the oil in aqueous emulsions with a hydrophilic Iipophilic balance (HLB) greater than the Ai I / ZiZSeilss value;

and 12, for example 12 to 20, such as 12 to 16, but alternatively may be suitable for stabilizing water in oil emulsions with an HLB value of less than 12, for example 1 to 8, and in particular 3 to 7. The composition of the invention may comprise a mixture of surfactants, for example as an emulsifier for said resin.

The surfactant may comprise at least one anionic, cationic, amphoteric and / or semipolar component.

Surfactants for use in the composition of the invention typically include hydrophobic groups such as alkenyl, cycloalkenyl, alkyl, cycloalkyl, aryl, alkylaryl 5 or more complex aryl (as in the petroleum sulphonates) of the 8 to 22 group, preferably 10 to 20, typically 12 to 18 carbon atoms, and a hydrophilic group. Other hydrophobic groups included in the compositions of the invention are polysiloxane groups. G

For example, the surfactant may consist essentially of at least a slightly water-soluble salt of sulfonic or monoesterified sulfuric acids, such as some alkylbenzene sulfonate, alkyl sulfate, alkyl ether sulfate, olefin sulfonate, alkyl sulfonate, alkylphenol sulfate, alkylphenol ether sulfate, alkylethanolamide sulfate, alkylethanolamide ether sulfate, or from some fatty α-sulfo acid or esters thereof having at least one alkyl or alkenyl group having from 8 to 22, more usually from 10 to 20, aliphatic carbon atoms. The term "ether" as used herein refers to compounds containing at least one glyceryl group and / or an oxyalkylene or polyoxyalkylene group, especially a group containing 1 to 20 oxyethylene and / or oxypropylene groups. In addition or alternatively, at least one oxybutylene group may be present. For example, the sulfonated or sulfated surfactant may be sodium dodecylbenzene sulfonate, sodium hexadecylbenzenesulfonate, sodium dodecyldimethylbenzenesulfonate, sodium lauryl sulfate, sulfonated tall oil sodium salt, potassium oleyl sulfate, ammonium lamonomethyl ammonium sulfate, or ethoxylated (10 mol) monoethanolamine cetyl sulfate.

Other anionic surfactants used in the composition of the present invention are alkyl sulfosuccinates such as sodium di- 6 - 2-ethylhexyl sulfosuccinate and sodium dihexyl sulfosuccinate, alkyphether sulfosuccinates, alkyl sulfosuccinamates, alkyl ether sulfosuccinamates, acyl sarcosinates, acyltaurides, isethionates, soaps such as atearates, palmitates, resinates, oleate, linoleate and alkyl ether carboxylates. Anionic phosphoric acid esters, alkyl phosphonates and alkylamine and -minomethylene phosphonates can also be used. In all cases, the anionic surfactant typically comprises at least one aliphatic-hydrocarbon chain having 8 to 22, preferably 10 to 20, carbon atoms, and, in the case of ethers, at least one glyceryl and / or 1 to 20 exyethylene and / or oxypropylene and / or oxybutylene groups. Preferred anionic surfactants are sodium salts. Other commercially preferred salts are potassium, lithium, ammonium, monoethanolamine, diethanolamine, triethanolamine and alkylamine salts with up to 7 aliphatic carbon atoms.

The surfactant used in the composition of the invention may optionally contain or consist of nonionic surfactants. For example, the nonionic surfactant may be a mono- or di- (lower) alkanolamine alkanolamide, such as coconut monoethanolamide. Other nonionic surfactants which may optionally be included in the present invention are tertiary acetylenic glycols, polyethoxylated alcohols, polyethoxylated mercaptans, polyethoxylated carboxylated acids, polyethoxylated amines, polyethoxylated alkylolamides, polyethoxylated alkylphenols, polyethoxylated coceryl esters, polyethoxylated sorbitan esters, polyethoxylated phosphoric esters, and propoxylated or ethoxylated and propoxylated analogs of all of the above ethoxylated nonionic compounds having an alkyl or alkenyl group and up to 20 ethylenoxy and / or propyleneoxy groups. Also included are copolymers of polyoxypropylene with co-ethylene oxide, copolymers of polyexybutylene with polyoxyethylene and polyoxybutylene-polyoxypropylene copolymers. The polyethoxy, polyoxypropylene and polyoxybutylene compounds may optionally contain end groups such as benzyl groups to reduce their foaming tendency.

The compositions of the invention preferably contain at least one mono-surfactant. am-

For example, the amphoteric surfactant may be a betaine, for example, betaine of the formula R 1 N CH 3 COO *, wherein R is alkyl, cycloalkyl, alkenyl, or alkaryl, and preferably at least one, and more preferably more than one substituent R has an average of 8 to 20, for example 10 to 18 aliphatic carbon atoms, and each of R 2 has an average of 1 to 4 carbon atoms. Particularly preferred are the quaternary betaine imidazole of the general formula

wherein R 1 and R 4 are alkyl, alkenyl, cycloalkyl, alkaryl or hydroxyalkyl groups having an average of 1 to 20 aliphatic carbon atoms. Preferably R has an average of 8 to 20, for example 10 to 18, aliphatic carbon atoms and R 1 preferably has 1 to 4 carbon atoms. Other amphoteric surfactants useful in the compositions of the present invention include alkylamine ether sulfates, sulfobetaines and other quaternary amine or quaternized imidazoline sulfonic acids and their salts, and other quaternary amine or quaternized imidazoline carboxylic acids and salts thereof and zwitterionic surfactants , for example, N-alkyltaurines, carboxylated amidoamines, such as those of the general formula RCCNHCHCHGJGR + CH 2 CH 2 Cl 2 Cl 2 CH 3 COO "', and amino acids always having hydrocarbon groups capable of imparting surfactant properties (e.g., alkyl, cycloalkyl, alkenyl or alkaryl groups with 8 to 20 aliphatic carbon atoms) Typical examples are 1-carboxymethylimidazoline with attached alkyl and amidoalkaleic tall oil residues and N-carboxymethyl-2- (hydroxyalkyl) imidazoline with coconut-bound alkyl radicals. Amphoteric or zwitterionic containing a surfactant compound that includes a hydrophobic moiety containing an ωθ alkyl or alkenyl moiety and a hydrophilic moiety containing an amine or quaternary ammonium group and a carboxylic sulfate or sulfone moiety can be used in the composition of the invention. - 8 -

The compositions of the invention may also include cationic surfactants.

The cationic surfactant may be, for example, an? -Cylammonium salt having a total of at least 8? Usually 10 to 30, for example 12 to 24 aliphatic carbon atoms, in particular a tri- or tetralkylammonium salt. Typically, alkylammonium surfactants for use in the compositions of the invention have one or at most two relatively long aliphatic chains (e.g., having a chain diameter of 8 to 20 carbon atoms, typically 12 to 18 carbon atoms) and two or three relatively short chain alkyl groups having in each case 1 to 4 carbon atoms, such as methyl or ethyl groups, preferably methyl groups. Typical examples are dodecyltrimethylammonium salts. Also suitable are benzalkonium salts having one alkyl group of 8 to 20 carbon atoms, two alkyl groups having 1 to 4 carbon atoms and a benzyl group.

Another class of cationic surfactants useful in the compositions of the present invention are the N-alkylpyridinium salts in which the alkyl group has an average of 8 to 22, preferably 10 to 20, carbon atoms. Similarly alkylated heterocyclic salts such as N-alkyl isoquinoline salts can also be used.

Also suitable are alkylaryldialkylammonium salts having an average of 10 to 30 aliphatic carbon atoms, for example those in which the alkyl-aryl group is an alkylbenzene group having an average of 8 to 22, preferably 10 to 20 aliphatic carbon atoms, and the two other alkyl groups usually have With 1 to 4 carbon atoms, such as methyl groups.

Other classes of cationic surfactants suitable for use in the compositions of the invention include alkylimidazoline or quaternized imidazoline salts having at least one alkyl group per molecule, on average 8 to 22, preferably 10 to 20 carbon atoms. Typical examples are alkylmethyl-hydroxyethylimidazolinium salts, alkylbenzylhydroxyethylimidazolinium salts and 2-alkyl-1-alkylamidoethylimidazoline salts.

Another class of cationic surfactants suitable for use in the compositions of the present invention include amidoamines, such as those formed by reacting an 8 to 22 carbon fatty acid or an ester, glyceride or similar amide to form a derivative thereof with a diamine or polyamine such as e.g. -loading ethylenediamine or diethylenetriamine in such proportions to keep at least one amino group free. Similarly, quaternized amidoamines can be used.

Typically, the cationic surfactant may be any water-soluble compound having a positively-inactivated group, usually containing a nitrogen atom and one or two alkyl groups each having an average of 8 to 22 carbon atoms.

The anionic moiety of the cationic surfactant may be any water-soluble anion, such as formate, acetate, lactate, tartrate, citrate, chloride, nitrate, sulfate or alkylsulfonate ion of up to 4 carbon atoms, such as methanesulfonate. Preferably, it is not a surfactant anion such as a higher alkyl sulfate or an organic sulfonate. Polyfluorinated anionic, nonionic or cationic surfactants are also suitable in the composition of the invention. Examples of surfactants are polyfluorinated alkyl sulfates and polyfluorinated quaternary ammonium compounds.

The compositions of the invention may contain a semipolar surfactant, such as an amine oxide, for example an amine oxide containing one or two (preferably one) C 8 -C 22 alkyl group, wherein the second substituent (s) is preferably a lower alkyl group, e.g. carbon atoms or benzyl groups.

It is also possible to use mixtures of two or more of the above-mentioned surfactants, in particular nonionic mixtures with cationic or amphoteric and / or semipolar surfactants or with anionic surfactants.

The surfactant is a conventional resin, but additionally a surface-active agent. present in the content emulsion - not added - 10 -

Typically, the compositions of the present invention contain 0.1 to 5%, for example 1.0 to 3.5% of a surfactant (or a mixture of surfactants), especially 0.2 to 1.5%, e.g. 4 to 1% of a surfactant added in addition to the surfactant present in the resin dispersion, which may be in an amount of 0.2 to 3.5%, for example 0.5 to 2.5%, based on the amount of components (i to i). The added surfactant may be 0.5 to 0.9% based on the amount of components (i to v). The emulsifier in the resin dispersion is preferably nonionic or anionic, for example an alkylsulfate / or alkyl ether sulfate.

The water-soluble ammonium polyphosphate (component vi), which is preferably present in the compositions of the present invention, is usually prepared by reacting condensed phosphoric acid with ammonia or an organic amine or quaternary ammonium hydroxide to form a water-soluble product. The condensed phosphoric acid typically has an average degree of condensation greater than 3, for example 3 to 30, and usually has a linear, branched or cyclic structure. Preferably, these salts contain nitrogen and phosphorus in an atomic ratio (0.5 to 2): 1, in particular about 1: 1. The polyphosphoric salt is preferably a mixture of ammonium salts of several polyphosphoric acids, which is obtained by reacting an aqueous solution of phosphoric acids containing 80 to 86% by weight. phosphorous pentoxide, with ammonia or a derivative thereof at a temperature of 15 to 70 ° C, for example 15 to 40 ° C, and at a pH of 4 to 12, for example 5 to 12, such as 5 to 9, 6 to 8 or 6.5 to 7.5 . Mixtures of ammonium polyphosphates that may be used are described in British Patent Specification No. 1504507 and can be prepared as described herein. Typically, this added ammonium polyphosphate has a (actual) water solubility of at least 50 g in 1 liter, such as at least 100 µl, at 20 ° C. Examples of suitable soluble polyphosphates include those blended with urea and manufactured by Albright and Wilson Ldt. Typically, the composition of the present invention comprises 0 to 10%, e.g. 2 to 8%, for example 4 to 6% of water-soluble polyphosphate monobasic.

The fabric flame retardant composition of the present invention generally comprises a carbamic acid derivative (component vii) having amino group 2 in the molecule, in a weight percent (as urea) and based on the amount of ammonium polyphosphonate in the range of 0.5. up to 300%, such as 0.5 to 50%, for example 5 to 30%, such as 7 to 20% or 10 to 20%. However, preferred ranges are 50 to 300%, e.g. 50 to 200% and especially 75 to 125%. The carbanic acid derivative may be guanidine or dicyandiamide, but is preferably also iodine. The amount by weight is considered to be urea, but it is possible to use an equivalent amount of another carbaraic acid derivative. The presence of a carbamic acid derivative reduces the possible tendency to discolor the fabric after heat curing. Typically, the composition of the present invention comprises from 0 to 10%, such as from 2 to 8%, for example from 4 to 6% of the carbamic acid derivative (expressed as urea).

The compositions of the invention are usually thixotropic pastes which can be cast when freshly prepared; they form a gel by standing, but can be converted into a liquid emulsion by spreading. The permanent emulsions may be of the water-in-oil type, but are preferably of the oil-in-water type. In contact with the cotton fabric solely by gravity, the compositions of the present invention do not tend to soak through the fabric or lose water rapidly by soaking it into the fabric. By rubbing the composition of the invention onto a fabric, for example under the pressure of a knife blade, the compositions of the present invention become fluid under the action of shearing forces so that they can penetrate into the fabric where they rapidly re-form the gel but do not penetrate the fabric and flow out of the opposite side. The compositions of the present invention may be prepared by mixing the ingredients in any order, usually in the order of first resin, then insoluble ammonium polyphosphate, followed preferably by a soluble ammonium polyphosphate and a carbamic acid derivative, followed by water and an antifoam agent. The mixing is usually carried out with a high speed stirrer.

Compositions of the invention containing components (i) to (iv) generally contain these in weight ratios (20 to 28): (0.01 to 5); (14 to 30): (50 to 60). Compositions of the invention containing components (i to vii) usually contain these in weight ratios (15 to .30): (0.01 to 5): (15 to 30): (40 to 51): (0.1 to 5): (2-8) :( 2-8). The substances to which the composition of the invention can be applied can be woven or non-woven. They are usually cellulose-based materials, for example pexulants such as cotton, linen, jute, jute - 12 - canvas, or regenerated cellulose materials such as silk or viscose, either alone or with other materials that can be mixed with them such as polyester, nylon, acrylic, acetate, polypropylene or silk fiber or wool. These compositions may contain at least 10%, or at least 20%, for example 15 to 100% or 30 to 90%, but preferably at least 40%, for example 40 to 75% of the cellulosic material. Preference is given to fabrics of homogeneously blended mixtures or of unmixed blends of cellulosic materials, such as cotton, with synthetic polymers such as polyester, nylon or acetylene.

Tulle fibers. The fibers used to form at least a portion of the fabrics may optionally have a core-shell structure, but preferably none. The fabrics may be of a unitary construction in which at least one of the weft material, and in particular the warp, is predominantly (e.g. fully synthetic polymer fibers. Preferred are those with a warp predominantly of polyester or nylon and a camouflaged weft, in particular an embossed cotton pattern and / or colored cotton fiber. The compositions according to the invention and the method of extending the flame retardancy of the fabrics according to the invention make it possible to provide more uniformly non-flammable treatment, at least temporarily, of more than one material, preferably an embossed pattern, but in particular with a non-uniform distribution of the synthetic polymeric and cellulosic material. their surface (in the other called "fabrics with different surfaces"). Particularly important tissues with different surfaces are those having a face with a different (usually lower) relative representation of the cellulosic material to the systhetic material than on the reverse side, as well as those having a face with considerable areas predominantly (for example 50 to 10%) of synthetic polymeric fiber fibers of the surface, as well as usually significant areas predominantly (e.g. 50 to 100%) of cellulosic material fibers. Examples of such fabrics with different surfaces are woven fabrics with polyester warp weave of dyed cotton, in particular weft of more than one differently colored cotton, or woven fabrics woven with face patterns of such dyed cotton on a background of a polyester warp and a non-patterned ruby side with a substantial proportion cotton surface. Such tufts with different surfaces can be used as fabric for furniture upholstery. Other suitable fabrics are pile-woven fabrics with cotton backing and a face with acrylic fiber. For fabrics of two or more materials and for woven fabrics, the composition of the invention is applied to the back of the fabrics. \ T

In addition to fabric for upholstery coatings, the composition of the present invention can be used for non-flammable treatment of other home textiles, such as curtains that are often not washed and which are suitable for use in, for example, home, office, office or public buildings. The ability to use the compositions of the invention to treat different types of fabrics is advantageous where different fabrics have the same or similar pattern that are used when a color-matched decor is to be achieved.

Flood specific gravity may range from 0.050 to 1.0 kg.m "2, for example 0.080 to 0.700 kg.m" 2, or 0.400 to 0.700 kg.m "2, 2 typically 0.200 to 0.400 kg.m, especially for fabrics containing at least 30% non-cellulosic fibers. Each of the fabric components may be yellow or uncoloured or may be colored especially in white or pastel shades. The fabric prior to impregnation is usually of dirt, starch, natural wax and applied finish, although it may contain an optical brightener.

The flame retardant composition of the present invention can also be used to impregnate carpets (by application to the back) which can have a specific weight of up to 2 kg.m.

The flame retardant composition of the present invention is typically applied at a pH of 2 to 8, for example 5.5 to 7.5, on a fabric substrate by applying it to the back side, for example by spreading a knife over a roller or pneumatically to achieve an application rate of 35 to 150% or 50%. up to 150% (based on the weight of the fabric), for example 60 to 80% for fabrics with; or 80 to 120% for fabrics of a homogeneous blend of fibers or for fabrics of two or more types of fibers. Typically, the minimum application rate required to achieve sufficient non-flammable treatment is that amount required to saturate the fabric (especially the pores in the fabric), or at least 95%, whichever is less.

After impregnation, the substrate may optionally be dried, for example, at a temperature of 80-120 ° C for 0.1-10 minutes. Drying can be carried out in any conventional drying apparatus, for example in a forced air dryer with forced air circulation or in a tensioning frame.

Optionally, the impregnated substrate is cured after drying, for example by heating at a temperature of at least 80 ° C, such as at least 120 ° C, for example 120 to 170 ° C, preferably 140 to 170 ° C or 140 to 165 ° C, for example 6 to half a minute, it is preferable to avoid combinations of longer periods with higher temperatures in order to reduce the tendency of the substrate to decolorize. Preferably, the drying and curing is carried out in one step.

Curing, which is usually continuous, can be accomplished by radiant heat heating, for example by infrared rays, but is preferably carried out by supplying hot air to the substrate surface, preferably to both surfaces, to ensure uniformity of heating. a dryer in which the hot air flows over the top and bottom surfaces of the substrate. The pad provides as uniform as possible with minimum burning. In the case of a washer dryer, the curing temperature of the substrate is substantially the same as that of the hot air flow. Typically, after curing, the substrate is cooled by introducing or letting cold air pass through it.

The finished cured fabric usually has a dry matter content of 30 to 60%, for example 35 to 45% for pile fabrics, or 50 to 60% for fabrics of wall or more types of fibers or for other fabrics without pile, and usually contains 3 to 10% phosphorus , preferably 5 to 5% phosphorus. The finished treated fabric has a flame retardancy versus untreated and can meet the BS 5852 test with ignition sources 0 and 1. The single-serve fabric in hard water at 40 ° C according to BS 5651 without final ironing can meet the flammability test of BS 5852 part1 with ignition sources 0 and 1. flame retardant treatment can hold 1 to 3 washings in soft water at a temperature of 74 ° C or 10 chemicals depending, in particular, on the type of resin composition of the composition.

Typically, the finished treated fabric has a substantially slight difference from the touch of the untreated fabric and shows no trace of deposited salts or resin on the surface. Usually the color does not differ from - 15 color untreated fabric.

The synergistic combination of components (i) to (iv), in particular with components (vj, cvi) and (vii), can give fabrics an improved non-flame retardant, and in particular a face and backsheet fabric, without salt deposits or face resin. on the side when the composition is applied on the reverse side of the invention. It is believed that the water-soluble and water-soluble ammonium polyphosphate added to the asakak or as part of the water-insoluble polyphosphate migrates from the reverse side towards the face but does not. In this specification, all parts and percentages are by weight.

The invention is illustrated by the following examples in which the following fabrics were used:

Fabric A was a cotton and polyester fabric (50: 50) with cotton weft and polyester warp, with a specific basis weight of 0.240 kg.m

Fabric B was a cotton and polyester fabric (65:35) with a cotton weft and a polyester warp, with a specific basis weight of 0.470 kg.m * ''. In both cases, a composition of the invention was prepared and applied to a fabric on a support substrate by means of a knife to spread the composition on the surface and rub it into the fabric. The backing mat was cooled in this procedure, but did not get wet, indicating that the water did not leak to the underside of the fabric. The impregnated fabric was then heated in a stretching frame at 150 ° C for 90 seconds, which included both drying and curing. The hardened material was then subjected to a non-flammability test in both the conditioned state and the leaching in hard water at 40 ° C according to BS 5651, Part 1, without final ironing.

The solubility of insoluble ammonium polyphosphate in water, as described in the specification and in the examples, was determined by an Ilander test in which 5 g of solid salt was shaken with 50 ml of water at room temperature and then 1C of the solution was decanted, weighed and evaporate to dryness leaving a residue. The solubility is expressed as ten times the weight of the residue after evaporation in grams. EXAMPLES Example 1

The composition of the invention is prepared by thoroughly mixing the listed ingredients, respectively, with 48 parts aqueous, 45.5% dry matter containing emulsions of a crosslinked, thermosetting acrylic copolymer containing an acrylonitrile monomer unit whose Tg is -24 ° C, marketed as REVACRYL 274 by Harris Chemical Co., England (an emulsifier comprising an alkyl ether sulfate and an alkyl benzene sulfonate is also present in the emulsion); 20 parts in water-insoluble ammonium polyphosphate, 98% of particles finer than 32 microns, containing 30.2% phosphorus and a solubility of about 3.5 g in 100 g of water at 20 ° C; 4.9 parts of urea; 4.9 parts of water-soluble ammonium polyphosphate prepared according to British Patent No. 1504507; 8.4 parts of water; and 0.1 parts of a 50:50 mixture of silicone oil (polydimethylsiloxane) with a hydrophobic silica-based antifoam agent manufactured by Wacker-Chemie GmbH under the designation S132. The insoluble polyphosphate is prepared by grinding the product manufactured by Albight and Wilson Limited under the name AMGARD KC.

The resulting composition was a liquid, stable emulsion that turned into a gel, which was re-converted into an emulsion by trituration; applied to fabric A at an application rate of 90%.

The cured fabric samples complied with the flammability test with ignition sources 0 and 1, and no traces of sedimentation resins were found on either the surface to which the composition was applied or on the opposite surface. Omal fabric was virtually unaffected by the finish. Example 2

The procedure was similar to Example 1, but the non-soluble ammonium polyphosphate was replaced by 24 parts of ammonium insoluble polyphosphate having a phosphorus content of 27.1% with an ICC% of particles less than 32 µm and a solubility of 6.32 g in IC 50 g water. . The resulting composition was used at an application rate of 94%.

The cured fabric samples ly again passed the flame retardancy tests, - 17 had no salt traces or resin on the surface and had a practically unchanged feel. Examples 3 to 16

Fabric B samples were impregnated with the compositions of the inventive compositions of Examples 1 and 2, but containing 20-24 parts of insoluble ammonium polyphosphate having the following characteristics: * Examples of phosphorus content solubility particle size (100% less than) (%) (g / 100g) 3.4 27.1 6.32 30 / µm 5.6 26.7 5.55 32 / ura 7, 8 27.3 3.55 32 µm 9, 10 27.5 3.33 32 µm 11, 12 27.9 3.16 32 y> µm 13, 14 27.3 2.96 32 / µm 15, 16 27.9 2.58 32 / µm All cured samples again passed the tests for reduced flammability, no traces on the surface neither salt nor pryksyřici and practically unchanged touch.

Industrial usability

The fabric flame retardant compositions of the present invention are suitable for both woven and nonwoven cellulose fiber substrates such as cotton, or regenerated cellulose fibers such as viscose, as well as synthetic cellulose fiber fabrics. fibers, for example polyester, nylon, acrylic, polypropylene, etc. fibers.

Claims (21)

- «lUDr. ETοδ VŠETCČKAadvokát <1604 PRAHA 1, Žitná 25 < 1. A fabric flame retardant composition comprising at least partially water-insoluble ammonium polyphosphate, a foaming agent, a thermosetting resin, water, and optionally a surfactant, a water-soluble ammonium polyphosphate and / or a derivative carbamic acid. 2. Composition according to claim 1, characterized in that the at least partially water-insoluble ammonium polyphosphate has a water solubility of less than 1 g / 100 g in the Manders test, in particular 0.5 to 3 g / 100 g, at 20 ° C. a mean particle size of less than 50 microns, in particular 10 to 20 microns, at least 60% of particles smaller than 30 microns, especially at least 40% of particles smaller than 10 microns, a molecular weight in the range of 1C00 to 2,000,000 and a phosphorus content of 20 % to 35 wt. 3. A composition according to claim 1 or 2, wherein the composition comprises 15 to 30 wt. at least partially in the water-insoluble ammonium polyphosphate, in particular 24 to 27%, when the surfactant, water-soluble ammonium polyphosphate and carbamic acid derivative are missing in the composition, or 19-23% by weight if these components are present in the composition. 4. A composition according to any one of claims 1 to 3 wherein the antifoaming agent comprises a soap, an alkyl ester of phosphoric acid or a formulation based on mineral oil, wax, vegetable oil or silicone, in particular a formulation comprising polysilosan, for example polydimethylsiloxane, and finely powdered silica. 5. A composition according to any one of claims 1 to 4, wherein said composition comprises 0.1 to 5 wt. anti-foaming agents. 6. A composition according to any one of claims 1 to 5 wherein the thermosetting resin is an acrylic copolymer comprising acrylonitrile monomer units, a copolymer of vinyl acetate with ethylene, a carboxylated acrylic copolymer with vinyl chloride, or a copolymer of ethyl acrylate. · 7. A composition according to any one of claims 1 to 6, characterized in that it contains 10 to 30 wt. if the surfactant, the water-soluble ammonium polyphosphate and the carbamic acid derivative are absent, or 20 to 25% by weight if the components are present in the composition. 8. A composition according to any one of claims 1 to 7 which comprises 0.1 to 5 wt. surfactants. 9. A composition according to any one of claims 1 to 8 wherein the water-soluble ammonium polyphosphate has at least one of these properties, namely an actual water solubility of greater than 50 g in 1 liter at 20 ° C, a ratio of the number of nitrogen atoms to the number of atoms phosphorus (0.5 to 2): 1, in particular about 1: 1, and an average degree of condensation of 3 to 30. 10. A composition according to any one of claims 1 to 9, wherein the composition comprises less than 10% by weight, in particular 4 to 6% by weight, of water-soluble ammonium polyphosphate. 11. A composition according to any one of claims 1 to 10 wherein the carbamic acid derivative is urea, especially when the composition contains less than 10%, and in particular 4 to 6%, by weight of the carbamic acid derivative. 12. A composition according to any one of claims 1 to 11, wherein the weight fraction of water-soluble ammonium polyphosphate, based on the weight of the carbamic acid derivative, is 0.5 to 300%, in particular 75 to 125% by weight. 13. A composition according to any one of claims 1 to 12 wherein at least partially water-insoluble ammonium polyphosphate, an anti-foaming agent, heat curable resin and water are present in the composition by weight (20 to 28): - 20 (0%). , 01 to 5}: (14 to 30): (50 to 60). 14. A composition according to any one of claims 1 to 12 wherein the amount by weight of at least partially water-insoluble ammonium polyphosphate, anti-foaming agent, thermosetting resin, water, surfactant, water-soluble ammonium polyphosphate and carbamic acid derivative is (15 to 30): (0, Cl to 5): (15 to 30): (40 to 51): (0.1 to 5): (2 to 8): (2 to 8). 15. A method of retarding fabric burning, wherein the fabric is impregnated with the composition of items 1 to 14 and then cured by heat. 16. A method according to claim 15, wherein the impregnation is carried out by applying the composition to the fabric surface, wherein a shear force is applied to the deposited material to inject it into the fabric, particularly when the application of the composition and the application force is performed in a single combined step, especially when this single process is performed using a knife applicator. 17. A method according to claim 15 or 16, wherein the fabric comprises cellulosic and non-cellulosic components, in particular from 40 to 75% by weight. cellulozovéhomateriálu. 18. A method as claimed in any one of claims 15 to 17 wherein a fabric of two or more components or fabrics is used with different surfaces, such as a woven fabric on one surface. 19. The method of claim 18, wherein the woven fabric is woven and the application rate is in the range of from 60 to 80% by weight. 20. The method of claim 18 wherein the fabric is made of two or more materials and the application rate is in the range of from about SC to about 12C% by weight. HHRHIHSHRHHnHfliiSiiilffiMM - 21 - 21. The method of claims 14 to 19, which comprises at least one of these parameters, namely, the weight of the fabric is within the range of 0.05 to 2 kg.m ", the curing is carried out at 120 ° C. to 170 ° C for 6 to half a minute, the hardened fabric has a dry matter content of 30 to 60% by weight, and the treated fabric contains phosphorus in an amount of 3 to 10% by weight.