Classifications

• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
  • C11D1/146—Sulfuric acid esters
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/37—Mixtures of compounds all of which are anionic
• • 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 ; Methods for using cleaning compositions
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents ; Methods for using cleaning compositions one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
• • 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/29—Sulfates of polyoxyalkylene ethers

Definitions

• the invention relates to heterogeneous surfactant granules with a inner grain consisting of longer chain alkyl sulfates or their mixtures with shorter-chain homologues or alkyl ether sulfates and a coating of shorter chain alkyl sulfates.
• Another object of the invention is a method directed to the production of the heterogeneous surfactant granules.
• Anionic surfactants especially alkyl sulfates or fatty alcohol sulfates, represent important components of washing, rinsing and cleaning agents.
• non-ionic Surfactants that have an inverse solubility behavior and due to hydrogen bonding in cold water are more soluble than in warm, anionic behave Conventional surfactants, i. H. their solubility increases by Reaching the solubility product more or less linear with the temperature too.
• anionic Surfactants that are adequate even in cold water Possess solubility.
• the best-known hydrotropes undoubtedly include the short-chain alkylarylsulfonates, such as, for example, toluene, xylene or cumene sulfonate. They are suitable, for example, as solubilizers for anionic and nonionic surfactants in the production of liquid detergents.
• the improved solubility is probably due to advantageous mixed micelle formation.
• German patent application DE-A1 4030688 (Henkel). It is proposed here to dry aqueous surfactant pastes using hot steam. Condensation of the superheated steam on the cooler feed and release of the heat of condensation to the material to be dried results in the surfactant droplets heating up spontaneously to the boiling point of the water. As a result, a multitude of fine channels form in the tenside grain when the water escapes. The resulting high internal surface area - for example compared to conventional spray-dried products - leads to a significantly improved dissolution rate. Nevertheless, there is the disadvantage that the method described is associated with a high level of technical complexity.
• solid detergents with high bulk density and improved solubility are obtained by adding mixtures of anionic and nonionic surfactants to polyethylene glycol ethers with a molecular weight in the range from 200 to 12,000, preferably 200 to 600, and then drying and / or in solid form.
• the rate of dissolution of the resulting solid detergents is still unsatisfactory.
• the presence of the large amounts of polymer required is not desirable.
• spray-dried detergent compositions are disclosed in general form which, in addition to anionic surfactants, contain nonionic surfactants, polyacrylates and polyethylene glycol ethers with an average molecular weight in the range from 1,000 to 20,000.
• the teaching of this document is that the dispersibility of anionic surfactants can be improved by adding nonionic surfactants, polyethylene glycol ethers and polyacrylates to them.
• DE-OS 2124526 relates to detergent and cleaning agent mixtures with controlled foam behavior .
• compositions which contain tallow alcohol sulfate, alkylbenzenesulfonate and polyethylene glycol with a molecular weight of approximately 20,000.
• solid detergents are known from international patent application WO 92/09676 (Henkel), which are obtained by treating aqueous alkyl sulfate pastes with soda and zeolites and then extruding them. The document does not reveal anything about the dissolution rate of the solids.
• Such detergents and cleaning agents are by Homogenization of the ingredients in a blender and subsequent treatment with additives such as Fatty alkyl sulfates produced.
• additives such as Fatty alkyl sulfates produced.
• the object of the invention has now been to create new forms of offer of alkyl sulfates to provide which are light colored even after mechanical compression and in show improved solubility in cold water.
• heterogeneous alkyl sulfate grain can then be obtained with further improved solubility if you have an inner grain, which is the longer chain Alkyl sulfate, optionally in a mixture with shorter-chain ones Contains homologues or selected alkyl ether sulfates Granulation with a coating of a short chain alkyl sulfate defined layer thickness.
• the sulfation products are among alkyl sulfates and alkyl ether sulfates primary alcohols or their ethylene oxide adducts to understand.
• Alkyl sulfates with 16 to 18 carbon atoms are considered have particularly advantageous washing properties.
• Typical Examples include cetyl sulfate and steryl sulfate and preferably tallow alkyl sulfate or technical mixtures comparable composition.
• component a) can be 100% by weight make out inner grain.
• a mixture is preferred used in addition to component a) either shorter-chain Alkyl sulfates with 12 to 14 carbon atoms (component b1) and / or alkyl ether sulfates with 16 to 18 carbon atoms and 1 to 3, preferably about 2, ethylene oxide units (Component b2).
• the weight ratio is between the components a) and b) usually in the range from 70:30 to 98 : 2 and is preferably 80:20 to 90:10.
• the coating of the inner grain again consists of shorter-chain ones Alkyl sulfates with 12 to 14 carbon atoms. Typical Examples are lauryl sulfate, myristyl sulfate or technical Mixtures based, for example, on a coconut fatty alcohol cut.
• the granulation is done in such a way performed that a coating with a layer thickness accordingly 0.5 to 10, preferably 1 to 5 and in particular 1.5 to 2 wt .-% based on the granules results.
• the substances that make up component a), ie the inner grain, alone or as a mixture, are used as dry powders.
• a dry tallow alkyl sulfate powder for example, an aqueous sulfuric acid half ester of a corresponding tallow alcohol can be subjected to spray neutralization following sulfation. It is also possible to dry a neutralized aqueous paste in a conventional spray tower or using superheated steam (see DE-A1 4124701 , Henkel). If a mixture of the C 16/18 alkyl sulfates with components b1) and / or b2) is desired as the inner grain, these can be prepared either mechanically by mixing the ingredients or by cosulfating the corresponding hydroxyl compounds.
• the sulfates are usually present as alkali metal salts and preferably as sodium salts.
• the granulation can be carried out in a manner known per se Mixer with drying device such as one Lödige mixers, Drais mixers, Schugi mixers or Fukai mixers or a fluidized bed continuously or discontinuously be performed.
• drying device such as one Lödige mixers, Drais mixers, Schugi mixers or Fukai mixers or a fluidized bed continuously or discontinuously be performed.
• the heterogeneous surfactant granulate is produced by coating a C 16/18 tallow alkyl sulfate powder with C 12/14 coconut alkyl sulfate using water as the granulating liquid.
• Granulation has also proven to be advantageous in such a way that particles result which predominantly, i.e. a diameter of at least 90% by weight have from 0.2 to 1.4 and preferably 0.2 to 0.8 mm. If necessary, coarse particles can be screened off.
• the surfactant granules according to the invention have rapid solubility in cold as in warm water as well as an improved Washing behavior in the washing machine. Another The advantage is that in the course of their mechanical compression no adverse effects on their color quality entry.
• the surfactant granules according to the invention can be combined with others Detergent ingredients mixed or agglomerated or are extruded and are accordingly suitable as Raw materials for the manufacture of solid detergents.
• Comparative example V1 was repeated. Instead of water, an aqueous paste of lauryl sulfate sodium salt with a solids content of 35% by weight (Texapon (R) LS35, Henkel KGaA, Duesseldorf / FRG) was used. The weight ratio between the inner grain and the coating was 1.5% by weight, based on the solids content of the granulating liquid.
• Texapon (R) LS35 Henkel KGaA, Duesseldorf / FRG
• Comparative example V1 was repeated. Instead of water, an aqueous paste of lauryl sulfate sodium salt with a solids content of 35% by weight (Texapon (R) LS35, Henkel KGaA, Duesseldorf / FRG) was used. The weight ratio between the inner grain and the coating was 2.5% by weight, based on the solids content of the granulating liquid.
• Texapon (R) LS35 Henkel KGaA, Duesseldorf / FRG
• Comparative example V1 was repeated. Instead of water, an aqueous paste of lauryl sulfate sodium salt with a solids content of 65% by weight (Texapon (R) LS65, Henkel KGaA, Düsseldorf / FRG) was used. The weight ratio between the inner grain and the coating was 1.5% by weight, based on the solids content of the granulating liquid.
• Texapon (R) LS65 Henkel KGaA, Düsseldorf / FRG
• An aqueous paste of C 16/18 tallow alkyl sulfate sodium salt with a solids content of about 50% by weight was subjected to conventional spray drying.
• the anhydrous powder was mixed in a weight ratio of 90:10 with a spray-neutralized powder of C 12/14 cocoalkyl sulfate sodium salt and then with the addition of an aqueous paste of lauryl sulfate sodium salt with a solids content of 35% by weight (Texapon (R) LS35, Henkel KGaA, Düsseldorf / FRG) granulated in a Lödige mixer.
• the weight ratio between the inner grain and the coating was 1.5% by weight, based on the solids content of the granulating liquid.
• Example 5 was repeated, but instead of the coconut alkyl sulfate, C 16/18 tallow alcohol 2EO sulfate sodium salt was used.
• a spray-dried mixed powder consisting of C 16/18 tallow alkyl sulfate, C 12/14 coconut alkyl sulfate and C 16/18 tallow alcohol 1EO sulfate (each in the form of the sodium salts, weight ratio 35:25:40) was added in a Lödige mixer granulated aqueous paste of lauryl sulfate sodium salt with a solids content of 35 wt .-%.
• the weight ratio between the inner grain and the coating was 2% by weight, based on the solids content of the granulating liquid.
• Example 5 was repeated, instead of the spray-dried one Tallow alkyl sulfate, however, steam-dried material used.
• the particle size of all granules examined was one Proportion of at least 90% by weight in the range from 0.2 to 1.4 mm.
• Tallow alkyl sulfate in the inner grain cKAS concentrate.
• coconut alkyl sulfate " cTAES concentrate.
• Example 5 was repeated, but granules of different particle size distribution were produced by varying the mixer speed, mass flow and mixing time.
• the results are summarized in Table 2: Hand washing tests: influence of particle size E.g. Particle size distribution Residue% -rel. ⁇ 0.2 mm 0.2-1.4 mm > 1.4 mm % By weight % By weight % By weight 8th 2nd 90 8th 25.7 9 1 93 6 25.1 V2 5 85 10th 28.2 V3 7 82 12th 31.0

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• 1994
  • 1994-05-02 DE DE4415369A patent/DE4415369C1/de not_active Expired - Fee Related
• 1995
  • 1995-04-24 US US08/732,422 patent/US5824633A/en not_active Expired - Fee Related
  • 1995-04-24 WO PCT/EP1995/001544 patent/WO1995029981A1/de active IP Right Grant
  • 1995-04-24 ES ES95918598T patent/ES2136851T3/es not_active Expired - Lifetime
  • 1995-04-24 DE DE59506594T patent/DE59506594D1/de not_active Expired - Fee Related
  • 1995-04-24 EP EP95918598A patent/EP0758374B1/de not_active Expired - Lifetime

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