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
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/39—Organic or inorganic per-compounds
  • C11D3/3902—Organic or inorganic per-compounds combined with specific additives
  • C11D3/3905—Bleach activators or bleach catalysts
  • C11D3/3935—Bleach activators or bleach catalysts granulated, coated or protected
• • 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

Definitions

• Bleach activators already react in the washing powder mixture, favored by the residual moisture present, with the bleaching agent, e.g. Sodium perborate if both components are unprotected.
• the bleaching agent e.g. Sodium perborate
• one of the two components is coated with a water-soluble agent that dissolves in the wash water during the washing process and releases the active substance.
• the bleach activator is preferably coated.
• water-soluble agents e.g. surfactants solid at room temperature, as described in EP-A-62523, or starch or cellulose derivatives as described in EP-A-37026.
• the activator powder is first premixed completely or partially dry with the auxiliary. In a second stage, this mixture is then moistened with water or with an aqueous solution of the remaining amount of the auxiliary and granulated.
• the activator granules are produced by extrusion of a mixture of activator and surfactant.
• FR-A-2 109 941 describes a process for the preparation of storage-stable, soluble bleach activator granules by coating the activators with a powdery auxiliary, in which the activator powder is moistened with water and then mixed and granulated with the powdered auxiliary.
• Water-soluble, calcined mineral salts, salt mixtures, powdery minerals or water-insoluble, powdery compounds with a large surface area, such as polyethylene or polypropylene, are used as powdery auxiliaries. 50 to 95% by weight of the auxiliary, based on the dry activator powder, are mixed into the moist activator powder.
• the present invention thus relates to a process for the preparation of a storage-stable, easily soluble bleach activator granulate by coating the activator with an auxiliary agent, the wettable powdery activator being first moistened with water, then the auxiliary agent being mixed as a powder with the moist activator and this mixture being granulated , characterized in that water-soluble cellulose ethers, water-soluble starch or water-soluble starch ethers are used as powdery auxiliaries.
• Suitable bleach activators for the process according to the invention are the known N-acylated amines, diamines, amides and glycolurils, preferably tetraacetylethylenediamine and tetraacetylglycoluril, as well as pentaacetylglucose and isononanoyloxybenzenesulfonate sodium. These activators are produced as a powder. In order to ensure a good dissolution of the activator in the wash liquor, it has proven to be useful to prefer to use those activators which have an average grain diameter of approximately 0.05 to 0.5 mm, in particular 0.07 to 0.2 mm exhibit. The desired average grain diameter can be achieved by sieving with calibrated sieves. However, the method according to the invention is not limited to the processing of particles of the specified grain sizes.
• the amount of water which is applied to the activator in the first cut by customary methods, for example by spraying, should be such that a moist, still Granules not prone to caking are formed.
• the activator powder is moistened with water in a ratio of 20: 1 to 4: 1, preferably in a ratio of 9: 1 to 5: 1 with water.
• a dye or white pigment can be added to the dry activator or the water to color it or to cover the natural color of the raw materials.
• a dye or white pigment can be added to the dry activator or the water to color it or to cover the natural color of the raw materials.
• generally 0.01 to 0.1 percent by weight, based on the finished product, of dye or pigment is sufficient.
• Suitable auxiliaries for this purpose are water-soluble cellulose ethers, water-soluble starch or water-soluble starch ethers.
• cellulose ethers are methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, methyl hydroxyethyl cellulose, methyl hydroxypropyl cellulose, carboxymethyl cellulose (as sodium salt) and methyl carboxymethyl cellulose (sodium salt).
• depolymerized starch can be considered as starch.
• Suitable starch ethers are, for example, carboxymethyl starch, hydroxyethyl starch and methyl starch.
• Sodium carboxymethyl cellulose has proven to be particularly suitable. All of these products are mixed in dry form with the activator.
• the moist activator is mixed with the powdery, dry auxiliary in conventional mixing devices. About 2 to 20% by weight of auxiliaries, based on the dry activator powder, are mixed into the moist activator powder.
• powdery disintegrants customary in the tablet industry can also be added, provided that they are used Cellulose and starch ethers do not in themselves have a certain explosive effect.
• Usable disintegrants are, for example, partially degraded starch, starch ether, polyvinyl polypyrrolidone, formaldehyde casein and swellable magnesium aluminosilicates. The proportion of such disintegrants can be 0 to 2 percent by weight of the finished granulate.
• the mixture thus obtained is then granulated in a suitable granulating device, for example in a granulating drum, in a high-speed mixer or on a granulating plate.
• a suitable granulating device for example in a granulating drum, in a high-speed mixer or on a granulating plate.
• Devices for press granulation such as extrusion presses or ring roller presses, are also suitable.
• the water content of the mixture is then reduced to less than 2, preferably less than 1 percent by weight.
• the excess water can be removed by drying with the addition of heat, the temperature of the granules advantageously not exceeding 100 ° C. and below the melting temperature of the bleach activator.
• the dried granules should contain less than 2, preferably less than 1 percent by weight of water.
• the granulate is intended for later use in detergents or is to be used for washing purposes, in which a certain content of such salts does not interfere, which are normally used in detergents or in washing processes and which can crystallize with the absorption of water of crystallization, the The excess water is also removed by mixing the moist granules with such dehydrating, essentially anhydrous or low-water salts.
• dehydrating essentially anhydrous or low-water salts.
• such salts are sodium tripolyphosphate, sodium sulfate, sodium carbonate, sodium silicate and low-water sodium aluminosilicates capable of ion exchange and mixtures thereof.
• the amount to be used depends on the Water binding capacity of the salts in question and the water content of the moist granules.
• the mixing ratio of tripolyphophate to moist granules is 1: 3 to 1: 1.5, in particular 1: 2 to 1: 1.
• Mixing can be carried out in conventional mixers or granulating devices, it also being possible to continue to use the mixing devices used for the production of the moist granules and equipped with mixing elements. In this way, simplified, in particular energy-saving, processing is possible since the necessary drying stage can be saved.
• the bleach activators obtained in this way, coated with an auxiliary agent, show a significantly better stability during storage in comparison to the activators of an analogous structure obtained by the process of EP-A 37026.
• TAED tetraacetylethylene diamine
• the resulting moist granules were dried in a fluid bed dryer to a residual moisture of approx. 1%.
• the granulate subsequently discharged from the dryer contained approximately 3.5% portions above 1400 ⁇ and approximately 26% below 500 ⁇ .
• the gut grain (portions between 500 ⁇ and 1400 ⁇ ) was sieved off and 3% mixed into a standard washing powder mixture containing sodium perborate. After 30 days of storage at 38 ° C and 80% relative humidity, 79% of the initial activity was still detectable by titration.
• the powder mixture was made from 11.8 kg TAED and 800 g Carboxymethylcellulose moistened with 1.87 l water in 60 seconds.
• the resulting mixture was passed through a perforated plate with 1 mm holes and dried to a residual moisture of 0.2%.
• 3% of the granules obtained in this way were mixed into a standard washing powder mixture containing perborate and kept in a climatic cabinet at 38 ° C. and 80% relative humidity for 30 days. After that, only 66% of the initial activity was detectable by titrimetry.

Landscapes

• 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)
• Detergent Compositions (AREA)

Applications Claiming Priority (2)

Publications (2)

Family

ID=6369820

Family Applications (1)

Country Status (6)

Families Citing this family (14)

Family Cites Families (10)

• 1988
  • 1988-12-22 DE DE3843195A patent/DE3843195A1/de not_active Withdrawn
• 1989
  • 1989-12-19 JP JP1327467A patent/JP2766915B2/ja not_active Expired - Lifetime
  • 1989-12-20 DE DE58908690T patent/DE58908690D1/de not_active Expired - Fee Related
  • 1989-12-20 EP EP89123523A patent/EP0374867B1/de not_active Expired - Lifetime
  • 1989-12-21 US US07/454,163 patent/US5100576A/en not_active Expired - Fee Related
  • 1989-12-21 IE IE417489A patent/IE66736B1/en not_active IP Right Cessation
  • 1989-12-21 DK DK655689A patent/DK655689A/da not_active Application Discontinuation

Also Published As

Similar Documents

Legal Events