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
  • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
• • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
• • 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
  • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents 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
  • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents 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 the liquefied ingredients being sprayed or adsorbed onto solid particles
• • 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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O

Definitions

• the invention relates to a builder component with a very high bulk density and to detergents or cleaning agents which contain this component.
• Such crystalline layered silicates are described, for example, in European patent application EP-A-0 164 514.
• Preferred crystalline layered silicates are those in which M is sodium and x is 2 or 3.
• both ⁇ - and ⁇ -sodium disilicate Na z Si 2 O 5 .yH 2 O are preferred, wherein ⁇ -sodium disilicate can be obtained, for example, by the method described in international patent application WO-A-91/08171.
• ⁇ -sodium disilicate is commercially available under the name SKS 7 (R)
• ⁇ -sodium disilicate is available under the name SKS 6 (R) (commercial products from Hoechst AG, Federal Republic of Germany).
• SKS 7 (R) commercial products from Hoechst AG, Federal Republic of Germany.
• the crystalline layered silicates are used in the form of a granular builders component which contains at least 10% by weight of crystalline layered silicates and 5 to 90% by weight in water Form of ions of organic acids and / or inorganic or organic salts present, although the material used should not exceed an average size of 300 microns, and possibly contain other binders, surfactants and other common ingredients of washing or cleaning agents.
• a preferred way of producing this builder component is roller compaction, a compression pressure of 10 to 50 kN / cm roller length and preferably around 25 kN / cm roller length being used.
• Such builders components still have high pH values in 1% aqueous solution; however, since these components have a higher dissolution rate than the powder, the risk of local deposits on textiles and thus damage to textile fibers is reduced.
• Roll compacting of detergents or cleaning agents or individual components of detergents or cleaning agents is a state of the art. It is already known from European patent application EP-A-0 253 323 that builders such as zeolite and / or phosphate can be converted into granules with a high bulk density and very good application properties by roller compaction. The conditions under which roller compaction is usually carried out are described in detail in this prior art document. It is stated that the pressing pressure in the nip and the dwell time of the material in the area of the pressing pressure are to be set in such a way that a well-formed band of high density is produced.
• the high degree of compaction is desirable not only with regard to modern washing or cleaning agents with a high bulk density, but also with regard to an increased abrasion resistance of the granules.
• excessively high pressures impair the process reliability, since when used the material is plasticized on the rollers and can lead to sticking.
• This undesirable effect occurs when an increase in the baling pressure no longer causes further compression of the material and the one that has now been added
• Pressing force mainly caused the heating and plasticization of the material - for example, by partial melting of water-containing components. This is also the reason why roller compaction is usually carried out at temperatures that are not additionally increased externally, but at ambient temperature.
• the object of the invention was to further develop the method of roller compaction of builders components which contain crystalline layered silicates in such a way that a further improvement in the dissolving behavior of crystalline layered silicates or of builders components which contain crystalline layered silicates is achieved.
• the invention accordingly relates to a process for producing a builder component which contains at least 10% by weight of crystalline phyllosilicates of the formula NaMSi x O 2x + 1 .yH 2 O, where M is sodium or hydrogen, x is a number from 1.9 to 4 and y is a number from 0 to 20, by roller compaction at compression pressures of up to 50 kN / cm roller length, the crystalline sheet silicates and, if appropriate, other conventional detergent ingredients being compacted at roller temperatures between 35 and 120 ° C.
• the invention encompasses both a method for roller compacting solely crystalline layered silicates, that is to say without additives, and also mixtures of crystalline layered silicates and customary further ingredients of washing or cleaning agents. If mixtures of crystalline layered silicates and conventional ingredients of washing or cleaning agents are used, it is preferred that the content of the mixture of crystalline layered silicates is 50 to 99.5% by weight and in particular 60 to 90% by weight. Disilicates, especially ⁇ -sodium disilicate and / or ⁇ -sodium disilicate, are used as particularly preferred crystalline sheet silicates.
• Preferred mixtures which are used in roller compaction are those which contain crystalline phyllosilicates and salts of inorganic and / or organic acids, in particular polybasic acids, the content of the mixture of these salts preferably being 0.5 to 50 % By weight and in particular 10 to 40% by weight.
• Preferred salts of inorganic polybasic acids are sulfates and carbonates, with sodium sulfate being particularly preferred, while citrates with particular preference for sodium citrate are preferred over salts of organic polybasic acids.
• Preferred organic acids are adipic acid, succinic acid, citric acid and glutaric acid, citrate and one or more organic acids also being able to be used in particularly preferred embodiments.
• the roller compacting is carried out in a mixture which consists of 70 to 90% by weight of ⁇ -sodium disilicate and / or ⁇ -sodium disilicate and 10 to 30% by weight of sodium sulfate and / or sodium citrate.
• the mixtures to be compacted can contain, in addition to or instead of these salts of inorganic and / or organic acids, other customary ingredients of washing or cleaning agents. Which ingredients may be suitable for this purpose can also be found in international patent application W0-A-92/18594.
• mixtures which contain crystalline layered silicates and conventional builders such as phosphates and / or zeolites. It is particularly preferred that the zeolite content of the mixture is preferably 0.5 to 50% by weight and in particular 1 to 20% by weight.
• the finely crystalline, synthetic and bound water-containing zeolite used is preferably zeolite NaA in detergent quality.
• zeolite NaX and zeolite P and mixtures of NaA, NaX and P are also suitable, for example.
• the zeolite is preferably used as a spray-dried powder with an average particle size of less than 10 ⁇ m (volume distribution; measurement method: Coulter counter) and preferably contains 18 to 22% by weight and in particular 20 to 22% by weight of bound water.
• Mixtures which contain 0 to 20% by weight and preferably 0 to 10% by weight of further customary ingredients of detergents or cleaning agents can also be used in roller compacting.
• the substance mixtures are preferably mixed together in powder form. It is possible that liquid constituents can also be incorporated into the mixture of substances, but it is Roll compaction not required. On the contrary, it is even preferred that components of detergents or cleaning agents which are in liquid form at the processing temperature are not used; In particular, it is preferred that components of detergents or cleaning agents which are also in liquid form at room temperature are not used in amounts above 5% by weight, based on the mixture, and advantageously not at all.
• the mixtures of substances can be produced in conventional mixers or granulators. Pre-compaction of the powder is also possible.
• the roller pressing itself can, however, take place without or with a pre-compression of the premixed powdery material.
• the pair of rollers can be arranged in any spatial direction, in particular thus vertically or horizontally to one another.
• the mixture to be compacted or the sole powder of crystalline layered silicate is then fed to the roll gap either by gravity filling or by means of a suitable device, for example by means of a stuffing screw.
• the material to be compacted is then passed under pressure through the gap of a pair of two rollers running in opposite directions at approximately the same circumferential speed and compacted to form a plate-like or band-shaped material to be pressed, which is also referred to as a sling belt.
• Preferred press pressures are between 7 and 30 kN / cm roll length and in particular press presses between 10 and 25 kN / cm roll length.
• roller compaction of crystalline layered silicates or of solid substance mixtures which contain crystalline layered silicates can not only be carried out without problems at elevated temperatures, but that this increased temperature also improves the dissolving behavior of the crystalline layered silicates or the builders components further, which contain crystalline layered silicates.
• Roll temperatures between 40 and 100 ° C and in particular between 45 and 90 ° C are particularly preferred.
• Roll compacting has proven to be particularly advantageous, which is carried out at roll temperatures between 50 and 70 ° C. and at pressures between 12 and 20 kN / cm roll length.
• the shoulder strap is then subjected to a comminution process.
• This comminution or grinding can take place, for example, in a mill.
• the comminuted material is then expediently subjected to a screening process, coarse material being separated off and returned to the comminution device, while material which is too fine is added again to the batch of the powdery mixture or the powdered layered silicate and is again fed to the compacting in the nip.
• the sliver belt is preferably made by conventional grinding into granules with a particle size range from 0.05 mm to about 2 mm, preferably with a particle size range consisting of at least 70% by weight of granules with a particle diameter between 0.1 and 1.6 mm exists, adjusted, while fine-grain fractions with granule diameters below 0.05 mm are returned to the compacting and coarse-grained fractions with granule diameters above 2 mm are returned to the grinding.
• a granular builder component is obtained which has a bulk density between 800 and 1100 g / l.
• the granular builder components obtained which in this case preferably consist of 100% by weight of crystalline phyllosilicates, are selected in a subsequent step with further ingredients of washing or cleaning agents, preferably with impregnating agents, from the group of the ethoxylated ones nonionic surfactants, mixtures of nonionic and anionic surfactants, pasty aqueous nonionic and / or anionic surfactants, the water possibly being subsequently dried off, and the silicone oils and paraffin oils, in particular with nonionic surfactants.
• the builder components can then also be powdered off with powdery solids, in particular with powdery crystalline layered silicates.
• the invention relates to a washing or cleaning agent which contains the builders components according to the invention.
• these agents preferably contain the agents according to the invention Builders components in amounts of 10 to 70 wt .-% and in particular in amounts of 20 to 60 wt .-%.
• the detergents or cleaning agents contain further conventional inorganic and / or organic builders, contents of 25 to 50% by weight of the builders components according to the invention are particularly advantageous.
• the washing or cleaning agents can contain all the usual ingredients such as anionic, nonionic, amphoteric, cationic and / or zwitterionic surfactants, other builders such as zeolite and / or phosphates, phyllosilicates such as bentonites, polycarboxylates such as citrates etc., polymeric polycarboxylates such as salts of homo- or copolymers of acrylic acid, bleaching agents and bleach activators, graying inhibitors such as cellulose ether or polyvinylpyrrolidone, optical brighteners, dyes and fragrances, and enzymes and enzyme stabilizers. Foam inhibitors can also be included.
• other builders such as zeolite and / or phosphates, phyllosilicates such as bentonites, polycarboxylates such as citrates etc., polymeric polycarboxylates such as salts of homo- or copolymers of acrylic acid, bleaching agents and bleach activators, graying inhibitors such as cellulose
• the agents can consist of a base granulate or of a multicomponent mixture, whereby multicomponent mixtures can be advantageous.
• enzyme granules and, for example, bleach activator granules, but also foam inhibitor granules or individual constituents such as sodium carbonate, sodium silicate or polycarboxylate are subsequently mixed in.
• the individual components can be made by spray drying, granulation, extrusion or other conventional techniques.
• the agents have a bulk density above 650 g / l, preferably above 700 g / l.
• detergents or cleaning agents with bulk densities above 800 g / l can also be produced without these agents tending to separate.
• These agents are also suitable for concentrates with high surfactant contents.
• a high anionic surfactant content can be achieved by admixing a highly concentrated anionic surfactant compound obtained, for example, by spray drying, spray neutralization or by granulation and simultaneous drying in a fluidized bed, and a high nonionic surfactant content by admixing the builder components with high nonionic surfactant components. Washing or cleaning agents with 15 to 40% by weight, in particular with 18 or 20 to 35% by weight, anionic and nonionic surfactants are preferred.
• the invention Roll-compacted granules, preferably loaded with nonionic surfactants, are added to extruded granules, which may contain highly concentrated anionic surfactant compounds and are preferably low in nonionic to nonionic in particular.
• Crystalline layered silicates of the type SKS 6 (R) ( ⁇ -sodium disilicate, commercial product from Hoechst AG, Germany) or the mixtures of SKS 6 (R) and the inorganic or organic salts of polybasic acids given below were pressed on a WR 50 N roller press / 75 (Alexanderwerk AG, Germany) at the temperatures given below to form scales of approx. 1 mm thickness. After comminution into granules with an average particle size range of 0.1 to 1.6 mm, products with the bulk densities specified below were obtained. The dissolving speeds given in the table were determined for the sieve fraction 0.6 to 0.8 mm according to the following test:

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Crystallography & Structural Chemistry (AREA)
• Detergent Compositions (AREA)
• Silicates, Zeolites, And Molecular Sieves (AREA)

Applications Claiming Priority (3)

Publications (2)

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ID=6496503

Family Applications (1)

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• 1993
  • 1993-09-01 DE DE4329394A patent/DE4329394B4/de not_active Expired - Fee Related
• 1994
  • 1994-08-22 DE DE59404364T patent/DE59404364D1/de not_active Expired - Fee Related
  • 1994-08-22 JP JP7507915A patent/JPH09501979A/ja active Pending
  • 1994-08-22 EP EP94925465A patent/EP0716682B1/de not_active Expired - Lifetime
  • 1994-08-22 ES ES94925465T patent/ES2109726T3/es not_active Expired - Lifetime
  • 1994-08-22 KR KR1019960701046A patent/KR960705019A/ko not_active Application Discontinuation
  • 1994-08-22 WO PCT/EP1994/002778 patent/WO1995006708A1/de active IP Right Grant
  • 1994-08-22 AT AT94925465T patent/ATE159280T1/de not_active IP Right Cessation

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