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WO1996004973A1 - Procede ameliore de sechage par pulverisation de compositions aqueuses de matieres utiles entrant dans la categorie des agents mouillants et des produits de lavage et/ou de nettoyage - Google Patents

Procede ameliore de sechage par pulverisation de compositions aqueuses de matieres utiles entrant dans la categorie des agents mouillants et des produits de lavage et/ou de nettoyage Download PDF

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Publication number
WO1996004973A1
WO1996004973A1 PCT/EP1995/003094 EP9503094W WO9604973A1 WO 1996004973 A1 WO1996004973 A1 WO 1996004973A1 EP 9503094 W EP9503094 W EP 9503094W WO 9604973 A1 WO9604973 A1 WO 9604973A1
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WO
WIPO (PCT)
Prior art keywords
drying
dry powder
water
spray
tower
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP1995/003094
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German (de)
English (en)
Inventor
Wilfried Rähse
Kathleen Paatz
Dieter Jung
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of WO1996004973A1 publication Critical patent/WO1996004973A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02—Preparation in the form of powder by spray drying
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/10—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it
    • F26B3/12—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour carrying the materials or objects to be dried with it in the form of a spray, i.e. sprayed or dispersed emulsions or suspensions

Definitions

  • the invention relates to the known method of spray drying water-containing preparations of valuable substances or mixtures of valuable substances from the field of wetting agents, detergents and / or cleaning agents, in which the corresponding flowable aqueous preparations are sprayed in upright towers and mixed with an or countercurrent hot gas phase dried to dry powder and then discharged from the spray tower.
  • the type of process that is still common on an industrial scale works with hot fuel gases or hot air as a drying gas phase in a single pass through the spray tower.
  • Corresponding spray drying processes with a circulation of such hot gas phases are also known in the literature, in particular with the aim of achieving self-inerting of the gas phase and thus protecting the material to be dried.
  • a well-known problem area for spray drying lies in the fact that the fine-particle sprayed particles which dry out from the flowable aqueous preparation by dehydration frequently pass through a state of increased surface tack in the course of this drying process before the drying has progressed to such an extent that this non-sticky, free-flowing powder is obtained.
  • This intermediate stage there is an increased risk of undesirable caking of the sprayed material on the tower walls and / or undesired adhesion of the particles to one another.
  • These difficulties make it necessary to carefully coordinate the geometric configuration of the spray zone in order to adapt it to the process conditions - for example in mass throughput, the form of hot gas flow in cocurrent and / or countercurrent, possibly with the addition of swirl gas streams and the like.
  • Considerable expenditure has to be made both in the area of investment - in particular the size and dimensions of the spray tower - and in the practical area of drying in order to cope with the difficulties of undesired gluing or coating formation mentioned here.
  • thermoplastic materials and other sticky materials on the housing walls of spray dryers are known from the prior art (K. Kröll, drying technology, 2nd volume, dryer and drying process, 2nd edition 1978, Springer Verlag, p. 294).
  • the walls of the dryers for the corresponding goods are provided with air-flow-through jackets, or blown chambers are circulated on the inside, which blow off the powder with cold air.
  • a cool and dehumidified air stream can be fed into the dryer so that it sweeps along the walls as a downward cold air curtain.
  • the supply of cold air or a cold air curtain is carried out in particular for the usually conical discharge funnel at the lower end of the cylindrical drying tower.
  • the cold air is conducted via an annular channel arranged in the attachment area of the cone and an air distribution plate into the interior of a double jacket, the inner wall of which ends below the inlet at approximately a height in which the inner and outer walls come very close.
  • the cold air flows through the narrow annular gap and is forced by this arrangement to flow tangentially to the inner wall of the cone.
  • the invention is based on the object of proposing further simplifications and improvements for solving the problem area, which are derived from an intermediate surface stickiness of the drying good particles with caking or caking on the inner wall of the vessel with subsequent thermal damage to the good part concerned.
  • the solution to this problem according to the invention lies in the measure described below in detail, in which small amounts of very fine solid matter in the form of a dry powder are introduced into the interior of the spray drying zone and here in particular into the areas where there is a risk of sticking or caking.
  • This powder or powder-like auxiliary material covers a possibly still sticky outer surface of the material to be dried and thus removes its stickiness to such an extent that the undisturbed free-flowing properties of the material to be dried are ensured, particularly in the problem areas. This reliably prevents both caking of the good particles with one another and, in particular, caking of the good particles on the inner wall of the spray dryer.
  • the invention accordingly relates to the process for spray drying water-containing preparations of valuable substances and mixtures of valuable substances from the field of wetting agents, detergents and / or cleaning agents in an upright tower using hot gases which are driven in cocurrent and / or countercurrent as a drying agent.
  • the process is characterized in that, in addition to and separately from the water-containing valuable substance preparations, small amounts of a finely powdered material to be dried are introduced into the spray tower. This finely divided drying material used as an auxiliary is simply referred to below as "dry powder".
  • the invention relates to the application of this principle of the process to the drying of water-containing preparations of the valuable substances and valuable substances concerned here, using superheated, circulated steam as drying gas.
  • Fine-particle dry powders in the sense of the teaching according to the invention can have a wide variety of properties and can be of inorganic and / or organic origin. For their part, they can be water-soluble and / or water-insoluble. Details of this will be given below. In order to understand the teaching according to the invention, first of all, its physical nature when used in the drying tower and the form of its addition are decisive:
  • the solid material to be fed into the tower or the endangered tower area is in the form of fine powdered dry material. It is added to the interior of the spray dryer as an additional component, it being essential that the dry powder be separated from the water-containing ones Recyclable materials - not mixed with them - is introduced into the spray tower.
  • the sufficiently rapid distribution of the fine powder in the endangered area can be important.
  • this is achieved by introducing the dry powder used in a comparatively small amount into the interior of the dryer by means of a gaseous carrier.
  • different special configurations are possible, which can also be connected to one another.
  • the dry powder is added to the hot gas stream immediately before or before it enters the dryer interior. It may be preferable to introduce the dry powder into the drying tower by means of one or more auxiliary gas streams. It can be particularly expedient to provide such an entry into the tower inner zones, which are particularly at risk from sticking and / or caking.
  • the partial streams used here as carriers for the dry powder can be partial streams of the drying gas - in particular also partial streams of the superheated steam - but they can also be additional auxiliary gas streams. Such a case exists, for example, when the dry powder is added as an additive to the auxiliary fluid, which according to the teaching of the previously mentioned earlier application DE-P 4321 361.8 is fed into the area of the drying tower below the lowest superheated steam inlet.
  • auxiliary fluid from the teaching of the earlier application is further reinforced by the use of the dry powder in the sense of the teaching now given.
  • the radial flow of the auxiliary fluid with the simultaneous addition of fine dry powders according to the invention leads to a reduction in the risk of sticking of the good particles even in the interior of the spray drying room.
  • water-soluble and / or water-insoluble, finely divided solids of inorganic and / or organic nature can be used as dry powder.
  • Suitable powders are particularly suitable, which - fed in as a dry, free-flowing solid - are practically non-sticky and / or non-swelling under the drying conditions in the spray tower.
  • the dry powder can contain at least a proportion of finely divided free-flowing recyclable materials and / or mixtures of recyclable materials in the specified field of application of the wetting, washing and cleaning agents.
  • a first interesting embodiment has to be considered in particular:
  • Spray-dried powders are known to be randomly distributed in terms of their individual particle size. In the practice of the spray drying process, this generally leads to the very fine fraction of the dry material being discharged from the spray drying room together with the drying gas stream. It is generally necessary to separate these very fine fractions of the dried material from the hot gas stream, and this can be done by using filters or separating devices of the cyclone type.
  • the fine material fraction of the primary dry material obtained here can be used as dry powder in the sense of the teaching according to the invention and in particular can be returned to the spray drying zone with auxiliary fluids or partial gas flows.
  • Aerosils are made up of amorphous spherical particles which have a diameter of 10 to 20 nm and an inner surface of, for example, 100 to 400 m 2 / g. Aerosils have SiOH groups on their surface, which are linked to one another via relatively weak hydrogen bonds, which leads to the formation of scaffolds. Aerosils are, for example, sales products from Degussa, Hanau / FRG. For more information on their structure, see Seifen- ⁇ le-Fette-Wwachs, 94, 849 (1968).
  • a very finely divided inorganic water-insoluble auxiliary in the sense of the definition according to the invention for the dry powder are corresponding metal oxide compounds, in particular aluminum oxide in its various preparations.
  • the dry powders of the type described here - but also the examples of useful materials which are still mentioned - can be used in the commercially customary and in particular non-hydrophobicized embodiment.
  • dry powders are used, at least in part, which contain the corresponding materials in hydrophobicized form.
  • Hydrophobicized aerosils like the non-hydrophobicized material, are commercial products for a wide variety of uses.
  • materials which have been rendered hydrophobic can be particularly suitable for preventing the undesirable caking and / or sticking together of the valuable materials.
  • water-soluble organic and / or inorganic solid powders are also suitable as dry powders.
  • Soluble polymer compounds of natural and / or synthetic or semisynthetic origin such as xanthan, starch, cellulose powder and their derivatives such as methyl cellulose and / or carboxymethyl cellulose, in particular with low water retention, may be mentioned here as examples.
  • organic solid components can be very finely powdered compounds with a surfactant character.
  • examples include fine powder anionic surfactants. Because of their oleophilic molecular constituent, they can achieve comparable effectiveness qualities to the hydrophobized inorganic powders for facilitating and regulating the drying process.
  • very finely divided inorganic and / or organic mixture components from the field of wetting agents, detergents and / or cleaning agents can also be used.
  • Soluble builder components based on alkali metal silicates (the so-called water glasses), adjusting agents such as soda, sodium sulfate and the like may be mentioned here as examples.
  • the dry powders used according to the invention as auxiliaries generally have considerable BET surfaces.
  • Corresponding surfaces of the dry powder either directly occur in its synthesis in a manner known per se - see, for example, the aerosils with BET surfaces in the range from about 50 to 400% / g - or they can be used as dry powder by appropriate pretreatment coming material can be ensured.
  • Particularly suitable for such a pretreatment is the grinding of a material of initially larger particle size and correspondingly smaller surface area.
  • the amounts of the dry powder to be used in the spray drying in each particular case are firstly determined by the reliable formation of the inhibition according to the invention with regard to bonding effects. As a rule, this can be achieved with very small amounts of dry powder, which usually make up at most about 10% by weight and preferably at most about 2 to 5% by weight, based on spray-dried valuable material . In general, amounts of the auxiliary substance below 1% by weight, based again on spray-dried material, will suffice. At least that applies to highly effective dry powder, for example of the type of a hydrophobic aerosil. In other embodiments, the targeted use of these auxiliaries in larger quantities may also be desirable. Such cases occur, for example, when the dry powder itself is a desired component of the resulting dry material.
  • Builder components or surfactant components are mentioned here as examples.
  • the optimized amount to be used in each case is also determined from the technical effect sought according to the invention of not causing or triggering excessive and undesired discharge of the added solid fines with the hot gas stream into a secondary separation stage.
  • an optimization of the desired process result can be set taking into account the technical knowledge.
  • An example here is anhydrous, free-flowing sugar surfactant powder which is obtained by drying aqueous preparations of alkyl and / or alkenyl oligoglycosides and / or of fatty acid N-alkylpolyhydroxyalkyl amides, in particular in the presence of inorganic and / or organic salts and, if appropriate, other carrier substances become.
  • the teaching according to the invention changes the technical teaching of the cited earlier application to the effect that dry powders, for example aerosils, in particular in hydrophobicized form, are introduced into the spray tower during the spray drying of water-containing preparation forms of the surfactant components.
  • Ci2 / l6-cocoalkyl oligoglucoside DP 1.33 (Plantaren ( R ) APG 600) with the following characteristics:
  • Average size of the primary particles 16 nm
  • Tamped density approx. 50 g / 1
  • the Aerosil was sprayed from above through a solid nozzle onto the partially dried surfactant particles.
  • the powder served as a spacer between the particles and thus prevented unwanted agglomeration.
  • the otherwise extremely hygroscopic, adhesive surfactant powder could be discharged through the double pendulum flap as a very free-flowing powder.
  • the aerosil as an anti-caking agent largely prevented the unwanted caking in the tower.
  • the bulk density was 375 g / 1.
  • the residual moisture was 2.6%.
  • the final product contained 3% powder material.
  • Ci2 / i6 cocoalkyl oligoglucoside DP 1.33 plantars ( R ) APG 600 CS UP, Henkel and 50% by weight Ci2 / i8 fatty alcohol sulfate sulfopone ( R ) 1218, Henkel with the following characteristics:
  • Ci6-18 70-80%
  • the end product showed very good powder properties.
  • the bulk density was 350 g / 1.
  • Ci2 / i6 cocoalkyl oligoglucoside DP 1.33 plantars ( R ) APG 600 CS UP, Henkel and
  • a sodium carboxymethyl cellulose (CMC) A250 from Aqualon was used as the powdering agent.
  • the APG powder powdered with 5% CMC had a bulk density of 390 g / 1.
  • the APG dried in this way performed very well in the tests with regard to the powder properties (dust test, clump test, sieve analysis).
  • the spray-dried and simultaneously powdered surfactant powder was composed of 90% fatty alcohol sulfate and 10% water glass with respect to the dry substance.
  • the bulk density was 340 g / 1.
  • the residual moisture was 2%.
  • a water glass Porti1 A ( R ) was used for powdering.
  • the powder addition has been adjusted so that 30% water glass with respect to the dry substance is contained in the end product.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

Selon un procédé de séchage par pulvérisation de compositions aqueuses de matières utiles et de mélanges de matières utiles entrant dans la catégorie des agents mouillants et des produits de lavage et/ou de nettoyage dans une tour verticale, on utilise des courants parallèles ou des courants opposés de gaz surchauffés comme agents de séchage. Le procédé se caractérise en ce que l'on introduit séparément dans la tour de pulvérisation, outre les compositions aqueuses de matières utiles, des quantités minimes d'une poudre sèche finement pulvérisée soluble et/ou insoluble dans l'eau. L'utilisation d'une poudre inorganique rendue hydrophobe finement pulvérisée et insoluble dans l'eau est préférable. Ce procédé permet notamment de décharger plus facilement les matières utiles séchées de tours de pulvérisation exploitées avec de la vapeur d'eau surchauffée comme gaz de séchage.
PCT/EP1995/003094 1994-08-11 1995-08-03 Procede ameliore de sechage par pulverisation de compositions aqueuses de matieres utiles entrant dans la categorie des agents mouillants et des produits de lavage et/ou de nettoyage Ceased WO1996004973A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19944428388 DE4428388A1 (de) 1994-08-11 1994-08-11 Verbessertes Verfahren zur Sprühtrocknung wasserhaltiger Wertstoffzubereitungen aus dem Bereich der Netz-, Wasch- und/oder Reinigungsmittel
DEP4428388.1 1994-08-11

Publications (1)

Publication Number Publication Date
WO1996004973A1 true WO1996004973A1 (fr) 1996-02-22

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ID=6525398

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Application Number Title Priority Date Filing Date
PCT/EP1995/003094 Ceased WO1996004973A1 (fr) 1994-08-11 1995-08-03 Procede ameliore de sechage par pulverisation de compositions aqueuses de matieres utiles entrant dans la categorie des agents mouillants et des produits de lavage et/ou de nettoyage

Country Status (2)

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DE (1) DE4428388A1 (fr)
WO (1) WO1996004973A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10021539C1 (de) * 2000-05-03 2002-02-28 Henkel Kgaa Vorrichtung zur Sprühtrocknung von lösungsmittelhaltigen Zusammensetzungen

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH336319A (de) * 1955-01-07 1959-02-15 Karlsruhe Augsburg Iweka Verfahren und Vorrichtung zur Gewinnung von trockenem Grobpulver aus einer Flüssigkeit
GB1075161A (en) * 1964-04-17 1967-07-12 Kroyer K K K A process for preparing a dry free-flowing glucose product from a solution thereof
US3629951A (en) * 1970-07-31 1971-12-28 Procter & Gamble Multilevel spray-drying method
US3842888A (en) * 1969-12-15 1974-10-22 Colgate Palmolive Co Apparatus for introducing ingredients into a spray drying tower
EP0378498A1 (fr) * 1989-01-09 1990-07-18 Niro A/S Procédé et dispositif de séchage par pulvérisation pour produire des particules agglomérées stables

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH336319A (de) * 1955-01-07 1959-02-15 Karlsruhe Augsburg Iweka Verfahren und Vorrichtung zur Gewinnung von trockenem Grobpulver aus einer Flüssigkeit
GB1075161A (en) * 1964-04-17 1967-07-12 Kroyer K K K A process for preparing a dry free-flowing glucose product from a solution thereof
US3842888A (en) * 1969-12-15 1974-10-22 Colgate Palmolive Co Apparatus for introducing ingredients into a spray drying tower
US3629951A (en) * 1970-07-31 1971-12-28 Procter & Gamble Multilevel spray-drying method
EP0378498A1 (fr) * 1989-01-09 1990-07-18 Niro A/S Procédé et dispositif de séchage par pulvérisation pour produire des particules agglomérées stables

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10021539C1 (de) * 2000-05-03 2002-02-28 Henkel Kgaa Vorrichtung zur Sprühtrocknung von lösungsmittelhaltigen Zusammensetzungen
US6769200B2 (en) 2000-05-03 2004-08-03 Henkel Kommanditgesellschaft Auf Aktien Device for spray-drying solvent-containing compositions

Also Published As

Publication number Publication date
DE4428388A1 (de) 1996-02-15

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