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
  • C11D3/16—Organic compounds
  • C11D3/20—Organic compounds containing oxygen
  • C11D3/22—Carbohydrates or derivatives thereof
  • C11D3/221—Mono, di- or trisaccharides or derivatives thereof
• • 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
  • C11D13/00—Making of soap or soap solutions in general; Apparatus therefor
  • C11D13/14—Shaping
  • C11D13/20—Shaping in the form of small particles, e.g. powder or flakes
• • 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
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
• • 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
  • C11D3/04—Water-soluble compounds
  • C11D3/08—Silicates
• • 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
  • C11D3/16—Organic compounds
  • C11D3/37—Polymers
  • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C11D3/3757—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions
  • C11D3/3761—(Co)polymerised carboxylic acids, -anhydrides, -esters in solid and liquid compositions in solid compositions
• • 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
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/06—Inorganic compounds
  • C11D9/08—Water-soluble compounds
  • C11D9/10—Salts
• • 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
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/22—Organic compounds, e.g. vitamins
  • C11D9/225—Polymers
• • 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
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/22—Organic compounds, e.g. vitamins
  • C11D9/26—Organic compounds, e.g. vitamins containing oxygen
  • C11D9/262—Organic compounds, e.g. vitamins containing oxygen containing carbohydrates

Definitions

• the present invention relates to a method for preparing a granular detergent material. More in particular, it relates to a method for preparing said granules from a dusty detergent component, such as soap, builders, e.g. sodium tripolyphosphate, surfactants, e.g. alkyl benzene sulphonate, soda ash, and corrosion inhibitors, such as disilicate.
• a dusty detergent component such as soap, builders, e.g. sodium tripolyphosphate, surfactants, e.g. alkyl benzene sulphonate, soda ash, and corrosion inhibitors, such as disilicate.
• Soap is a common ingredient of detergent powder compositions. It may be included as a detergent active, a builder or a foam suppressor. It may be added to a slurry which is subsequently spray-dried, or dry-mixed with other particulate ingredients, including composite particles which are themselves the product of a spray-­drying process.
• soap When supplied as a raw material for incorporating in such compositions, soap is often in the form of a fine dusty powder. As well as being messy in the handling, such powders have a tendency to cause respiratory tract irritation in those working with them.
• US Patents 3,761,549 and 3,588,950 describe a process of making non-dusty granulates by means of gas fluidisation in a rotating drum.
• Granules which, it is said, can be made in this way include those with a core of potassium soap coated with sodium soap, a core of a strong caustic detergent coated with a mild caustic detergent or a core of potassium soap with a coating of metasilicate.
• the core is formed by interactions during the fluidisation process and the coating is applied by spraying-on the coating as a liquid.
• non-dusting soap granulates are formed by mixing soap dust with fatty acid and an alkaline material which saponifies the acid.
• the resultant particles consist of two kinds of soaps.
• non-dusting granules of a detergent component may be made in a simplified process, optionally in mixture with a wide variety of other materials.
• the detergent component can be worked into a substantially non-dusty form from a pre-mix comprising:
• This pre-mix is used to prepare a granular detergent material having a core of granulising particles coated with a detergent component and a binder, comprising up to 40% by weight of the detergent component and from 1 to 10% by weight of the binder.
• this granular detergent material can vary. However, it is believed that the granulising particles are coated with the detergent component and the binder.
• the dusty detergent component and the granulising particles are admixed intimately and the resultant product is then admixed with the binder to form said pre-mix. Mixing of the pre-mix then continues until the granular detergent material is formed.
• This granular detergent material is considerably less dusty than, for instance, known fine soap powders, yet the process defined above for its production is more cost-effective than extrusion techniques and the like.
• granulating as an adjective is used to refer to components which are capable of being processed to form compositions comprising granules.
• granulising is used to refer to particles which are capable of acting on other substances, during processing, to form those substances into granules.
• the granules obtained are, by themselves, suitable for incorporation in complete detergent powder compositions which also comprise one or more synthetic detergent actives selected from anionic, nonionic, cationic, zwitterionic or amphoteric surfactants.
• These complete compositions preferably also contain other ingredients usual in such powders, for example detergency builders (i.e. substances which sequester and/or precipitate calcium ions contributing to water hardness), soil-­suspending and anti-redeposition agents, corrosion inhibitors, buffers, bleaches (including low-­temperature systems comprising a bleach precursor and an activator therefor), enzymes, enzyme stabilisers, lather boosters or foam depressors, dyes, pigments, fluorescers and perfumes etc.
• detergency builders i.e. substances which sequester and/or precipitate calcium ions contributing to water hardness
• soil-­suspending and anti-redeposition agents i.e. substances which sequester and/or precipitate calcium ions contributing to water
• Soap-containing complete detergent powder compositions for which soap-containing granules according to the present invention are well suited to formulating include those generically and specifically described in patent specification EP-A-117,568.
• the base mixture also contains the granulising particles.
• the granulising particles should be of one or more substances which are usual ingredients in detergent powders such as recited in the preceding paragraph.
• One preferred class of granulising particles comprises neutral and alkaline salts of alkali metal cations and organic or inorganic anions, into which class fall many of the aforementioned "usual ingredients" (which will be mentioned in more detail hereinbelow).
• especially preferred salts are the alkali metal metasilicates (preferably hydrated), for example sodium metasilicate 5 aq. which is a corrosion inhibitor/­alkaline buffer.
• granulising particles whether salts or otherwise, as a general rule it is preferred that they should not be too pervious to water, which is why the salts should be hydrated.
• the granulising particles should also be capable of surviving without fragmentation in the mixing apparatus used ( vide infra ).
• the dusty detergent component may, in principle, be any usual detergent component.
• the process of the invention is particularly suited for soap; builders like sodium tripolyphosphate, zeolite or polyacrylates; surfactants, such as alkyl benzene sulphonate; soda ash; and corrosion inhibitors, such as disilicate. Especially good results are obtained for dusty soap powders.
• the detergent component may be of any kind, provided it is compatible with the binder, the granulising particles and the mixing apparatus. On the latter point, it is believed to be important that it should not soften too much or melt with the heat of mixing, although some softening may aid the granulation process.
• it will be added to the mixer in the form of the known fine dusty powders, in order to convert it to a more acceptable form. However, in some circumstances it may be possible to add them as larger particles or even lumps, depending on the type of mixer, the kind of detergent component and the working temperature.
• soaps which are capable of producing extremely good quality granules by this invention are tallow and hardened fish/rape soaps. In the case of softer soaps, better results may be obtained if the mixture is cooled during processing.
• the binder is any substance capable of bonding the fine detergent component particles to form and maintain granules thereof and to enable them to coat the granulising particles. Thus, it should be compatible with the detergent component and with the granulising particles. It should also possess a "setting property", either alone or by interaction with the detergent component. Especially useful are aqueous-based binders, in which the detergent component is at least partly soluble, for example aqueous solutions of sugars, polyacrylate polymers or neutral waterglass, the latter being most preferred, or water. Generally, these substances will be used at aqueous concentrations at which the liquid is viscous and 'sticky'. Thus, for example, waterglasses may be in solutions from about 25% to about 50% by weight, typically around 34% by weight. It is also possible to utilise gums and the like.
• the binder may also contain other ingredients such as dyes, optical brighteners and the like.
• ingredients mentioned above in respect of complete detergent powder compositions are the synthetic anionic, nonionic, cationic, zwitterionic and amphoteric surfactants. These will be well known to those skilled in the art and, for example, may be selected from the classes, sub-classes and individual agents described in "Surface Active Agents", Vol. I by Schwartz & Perry (Interscience 1949) and “Surface Active Agents", Vol. II by Schwartz, Perry and Berch (Interscience 1958).
• the preferred but optional other ingredients of the complete composition are the "usual ingredients". Most important of these are the detergency builders. Those which are crystalline, and in some cases amorphous, inorganic or non-polymeric organic salts may either be added to the complete detergent powder composition and/or constitute the granulising particles.
• This class includes water-soluble alkali metal phosphates, triphosphates, polyphosphates, silicates, borates, and also carbonates. Specific examples of such salts are sodium and potassium triphosphates, pyrophosphates, orthophosphates, hexametaphosphates, tetraborates, neutral silicates and carbonates.
• aluminosilicate is an amorphous water-insoluble hydrated compound of the formula Na x (AlO2.SiO2)y, wherein x is a number from 1.0 to 1.2 and y is 1, said amorphous material being further characterised by an Mg++ exchange capacity of from 50 mg eq. CaCO3/g to about 150 mq eg. CaCO3/g and a particle diameter of from about 0.01 micron to about 5 microns.
• This ion exchange builder is more fully described in British Patent Specification No. 1 470 250.
• a second such water-insoluble synthetic aluminosilicate ion exchage material is crystalline and has the formula Na z [(AlO2) y (SiO2)] xH2O, wherein z and y are integers of at least 6; the molar ratio of z to y is in the range from 1.0 to about 0.5, and x is an integer from about 15 to about 264, said aluminosilicate ion exchange material having a particle size diameter from about 0.1 micron to about 100 microns; a calcium ion exchange capacity on an anhydrous basis of at least about 200 milligrams equivalent of CaCO3 hardness per gram; and a calcium ion exchange rate on an anhydrous basis of at least about 2 gralns/gallon/minute/gram.
• These synthetic aluminosilicates are more fully described in British Patent Specification No. 1 429 143.
• Suitable organic builder salts in this class are:
• alkali metal salts of ethane-2-carboxy-1,1-diphosphonic acid include the alkali metal salts of ethane-2-carboxy-1,1-diphosphonic acid, hydroxymethane diphosphonic acid, carboxyl diphosphonic acid, ethane-1-­hydroxy-1,1,2-triphosphonic acid, ethane-2-hydroxy-­1,1,2-triphosphonic acid, propane-1,1,3,3-­tetraphosphonic acid, propane-1,1,2,3,-tetraphosphonic acid, and propane-1,2,2,3-tetraphosphonic acid.
• alkylmalonates, alkylsuccinates, alkylsulphocarboxylates and carboxymethyloxymalonates include the salts of the free acids or of esters thereof.
• Other polycarboxylate builders which can be used satisfactorily, include water-soluble salts of mellitic acid, citric acid, and carboxymethyloxy succinic acid and salts of polymers of itaconic acid
• polystyrene builders are the water-soluble salts of polycarboxylate polymers and copolymers as described in U.S. Patent Specification No. 3 308 067.
• oxygen bleaches such as alkali metal peroxygen compounds (perborates, percarbonates, etc.) as well as activators therefor.
• activators A large number of such activators is known, but one preferred agent in the context of this invention, especially as the granulising particles, is N,N,N′,N′-tetraacetyl ethylenediamine, otherwise known as TAED.
• the pre-mix and granular detergent material described above may be prepared, using any mixing apparatus according to the scale intended but the Lödige (Trade Mark) batch-type of mixers, for example the FKM-range, are especially preferred.
• the dusty detergent component and the granulising particles are admixed for about half to about 5 minutes (typically about 3); the binder is then added in an amount which by simple trial and error will be found to yield the best formed particles with minimum lumps present.
• a good guide is to add the binder slowly until the mix just takes on a slightly wet appearance. Below this concentration there is an increasing tendency for the granules to form imperfectly. Above this level, there is a progressive tendency for the mixture to stick to the knives of the mixer and eventually form lumps which contaminate the final product.
• mixing is continued for at least 3 minutes, most preferably for 5 or even 10 minutes, the best results being obtained after about 15 minutes or more.
• the binder is added in an amount of about 1 to about 10% by weight, but we have found that in most situations the optimum is in the range from about 5 to about 7%. Generally speaking, the more dusty detergent component is present, the more binder is needed. It is possible to granulate up to 40% by weight of detergent component in the total composition by this method, but normally this will be from about 25 to about 38%. In most situations, the balance of the pre-mix will consist only of the granulising particles, but optionally small amounts of other components may also be present.
• Granulising particles may be chosen from amongst a very wide range of particle sizes.
• average particle size means the diameter value in which 50% of the particles are larger and 50% are smaller. Of course, the particles will not be as small as the fine dusty detergent component referred to previously. In general, the average particle size will be from about 75 ⁇ m to about 4,000 ⁇ m, preferably from about 250 ⁇ m to about 2,500 ⁇ m.
• compositions were prepared by mixing of soap and granulising particles for three minutes in a Lödige M 20 (a batch-type of mixer), followed by addition of the binder and continued mixing for a further 15 minutes. In all cases the resulting product was a granular mixture. The products had the consistency shown. All amounts are percentages by weight.
• Particle Size Distribution (%) ⁇ 180 ⁇ m 21.1 >500 ⁇ m 16.6 >180 ⁇ m 13.3 >710 ⁇ m 11.2 >250 ⁇ m 28.4 >1000 ⁇ m 9.5
• Amounts are in percentages by weight.
• Examples 1-3 were repeated, using as the dusty detergent component a mixture of : Alkyl benzene sulphonate 18.0 Burkeite adjunct 20.0 Soap 4.0 Sodium carboxymethyl cellulose 0.5 Savinase (enzyme) 0.65 Perfume 0.35 Na-metasilicate 5 aq. 6.0 the granulising particles : STP 48.5 binder : Na-waterglass solution, 34% 2.0 A free-flowing mixture of granular particles was obtained having excellent powder properties.
• the dusty detergent component a mixture of : Alkyl benzene sulphonate 18.0 Burkeite adjunct 20.0 Soap 4.0 Sodium carboxymethyl cellulose 0.5 Savinase (enzyme) 0.65 Perfume 0.35 Na-metasilicate 5 aq. 6.0 the granulising particles : STP 48.5 binder : Na-waterglass solution, 34% 2.0 A free-flowing mixture of granular particles was obtained having excellent powder properties.
• Examples 1-3 were repeated, using dusty sodium tripolyphosphate (20.1%), sodium metasilicate.5 aq. (77.9%) as granulising particles and a 34% solution of sodium waterglass (2.0%) as binder. Granules having good powder properties were obtained.
• Examples 1-3 were repeated, using dusty alkylbenzene sulphonate (26.0%), sodium tripolyphosphate particles (72.5%) as granulising particles and a 34% solution of sodium waterglass (1.5%) as binder. Granules having good powder properties were obtained.
• Examples 1-3 were repeated, using dusty soda ash (15.0%), sodium metasilicate.5 aq. particles (79.1%) as granulising particles and a 34% solution of waterglass (5-7%) as binder. The properties of the granules obtained were good.
• Examples 1-3 were repeated, using dusty sodium disilicate (20.0%), STP granules (78.0%) as granulising particles and water (2.0%) as binder.
• the granules obtained had good powder properties.

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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)
• Health & Medical Sciences (AREA)
• Inorganic Chemistry (AREA)
• Molecular Biology (AREA)
• Emergency Medicine (AREA)
• Detergent Compositions (AREA)

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Cited By (5)

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• 1987
  • 1987-12-11 GB GB878728959A patent/GB8728959D0/en active Pending
• 1988
  • 1988-11-30 EP EP88202736A patent/EP0323659B2/fr not_active Expired - Lifetime
  • 1988-11-30 DE DE3852754T patent/DE3852754T3/de not_active Expired - Fee Related
  • 1988-11-30 ES ES88202736T patent/ES2067467T5/es not_active Expired - Lifetime
  • 1988-12-06 NZ NZ227224A patent/NZ227224A/en unknown
  • 1988-12-07 AU AU26674/88A patent/AU615239B2/en not_active Ceased
  • 1988-12-07 FI FI885665A patent/FI885665A7/fi not_active IP Right Cessation
  • 1988-12-09 ZA ZA889240A patent/ZA889240B/xx unknown

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