JPH07122073B2 - Aggregate for powder detergent addition - Google Patents

Description

The present invention relates to color-improving agglomerate compositions and in particular white agglomerates of clay fabric softeners for addition to white or other colored detergent base powders.

Powdered detergents without colorants are generally white or close to white in color, but depending on the formulation, some fabric softening clays, enzyme granules or bleach precursors may be brown, yellow or grayish in color. is there. The presence of such discolored particles in the finished detergent powder can also result in an unattractive, non-white appearance of the overall product.

GB2 199 338 (Unilever Plc) proposes to use brightly colored large particles ("speckles") in powder detergents to obscure the presence of slightly discolored particles. There is.

GB 2 121 843 (Colgate-Palmolive Co) proposes to form a clay mottle by incorporating a dye or pigment in the agglomeration spray liquid used for the production of bentonite clay agglomerates.

However, in some powder detergents the use of mottle may not be desirable or may not be effective in camouflaging discolored particles.

Surprisingly, the inventor is unable to change the reflectance with further increase in layer thickness, with a certain mean particle size, bulk density and reflectance (values measured as R infinity at 460 nm). Aggregates coated or granulated with brightener particles (representing the reflectivity of layers of such thickness) are particularly white and bright when added to detergent-based washing powders I found that there are many cases.

Therefore, the first aspect of the present invention is that the average particle size is less than 20μ, the bulk density is less than 400g /, and the reflectance is greater than 85 (R infinity 460).
And an aggregate comprising whitening agent particles of

A second aspect of the present invention provides a fabric softener comprising clay agglomerates, the agglomerates having an average particle size of less than 20μ and a bulk density of less than 400 g / reflectance greater than 85 (R infinity 460). Whitening agent particles.

A third aspect of the present invention provides that the aggregate has a value of R greater than 75.
Provide an agglomerate containing sufficient brightener particles to provide a reflectance of infinity 460.

The color-improved agglomerates of the invention can be formed as cogranulates with whitening particles or as agglomerates coated with whitening agent particles.

The co-granulated agglomerates preferably contain 30-60% by weight, more preferably 40-50% by weight of brightener particles.

The average particle size of the whitening agent particles is preferably less than 15μ, more preferably less than 10μ.

The bulk density of the whitening agent particles is preferably less than 250 g /.

The reflectance, measured as R infinity 460, is preferably greater than 95.

When the whitening agent particles are present as a coating on the agglomerates, they preferably constitute 10-40% by weight of the total agglomerate composition. More preferably, the brightener particles make up 15 to 25% by weight of the total aggregate composition.

The whitening agent particles are preferably precipitated calcium carbonate or silica. The precipitated calcium carbonate used may be in the form of trigonal or aragonite crystals with an average particle size of about 4μ.

The silica used is in the form of a precipitated amorphous powder with a particle size of about 10μ.

An extremely useful precipitated calcium carbonate for whitening aggregates is known as SOCAL U3 (from Solvay). A very useful silica for whitening aggregates is Microsil (Cr
made by osfields).

Clay softeners are well known in the detergent field in the patent literature. Examples of this type of clay softener include various heat treated kaolins and various multilayer smectites. GB1 400 898 (Procter and Gamble) proposes the use of smectite clay which has a relatively high exchange capacity. There is a desire to enhance the efficacy of clays for fabric softening during washing, and the inventor's copending patent application EP 287 3
According to No. 44, if a certain nonionic surfactant is supported on the clay at a specific ratio and the water content of the resulting composition is adjusted, the fabric softening performance is improved. Has been. It should be understood that the examples described herein below relate to clays carrying nonionic surfactants, but the invention is not limited to clays.

The water content of the clay aggregate is 7.5 to 12% by weight, preferably 8
It has been found that it should be ~ 10% by weight.
Regarding this point, in the present invention, "water content (water content)"
The term need not necessarily be the total water content, but rather the water lost from the composition to a constant weight upon drying in a static environment at 135 ° C. Usually,
When freshly prepared, the clay / nonionic surfactant agglomerates have a relatively high water content, eg 10-16% moisture, and are therefore too sticky to use and require some post-drying. Is. When post-drying clay / nonionic surfactant agglomerates with high water content, the temperature of the drying air is
It is recognized that 85-90 ° C is suitable. When coating the agglomerates with precipitated calcium carbonate, "overdrying" the agglomerates so that the water taken up by the agglomerates as a result of the coating process gives the agglomerates with a final moisture content in the desired range. Is desirable.

Nonionic surfactant system is 0 when the concentration is 1% in distilled water.
It is present as a cloudy phase in the temperature range of 80 ° C to 80 ° C, preferably 0 ° C to 15 ° C. Practically this means that the system has a cloud point below 80 ° C, preferably below 15 ° C. The cloud point closely correlates with the hydrophilic oil balance (HLB) of the surfactant system and thus preferably has an HLB of less than 13.5, such as 12.0 or less, ideally less than 9.5. The HLB should be above 6.0 and preferably above 8.0 to provide sufficient detergency.

Specific nonionic surfactants are alkyl (C ₆ ~C ₂₂₎ phenol - ethylene oxide condensates, aliphatic (C ₈ ~
C ₁₈ ) Condensates of primary or secondary straight chain or branched alcohols with ethylene oxide, and products formed by condensing reaction products of propylene oxide and ethylenediamine with ethylene oxide.

The clay softener can be any material that can provide a softening effect. The effectiveness of the clay material as a fabric softener will depend on the amount of smectite clay. 3: 1 to 20: 1 of clay and nonionic surfactant in the aggregate is preferable,
Most preferably, it is 4: 1 to 10: 1.

If the agglomerates may be handled by conveyors, feeders, mixers, fillers or exposed to transport shocks, a binder may be added during the granulation process if nonionic surfactants are added to them. It may be necessary to use to improve the structural stability of the aggregate. Suitable binders include polyacrylates and copolymers of maleic anhydride polyacrylates, sugars, nonionic surfactants, polyethylene glycols, polyoxyethylene alkyl ethers, fatty acid monoethanolamides, carboxymethylcellulose, soaps and latices.

The aggregate of the present invention can be usually produced by a known granulation method as described in GB2 121 843B. Cogranulated
The agglomerates can be prepared by any granulator capable of contacting the material to be agglomerated with the binder, Schugi Flexomi
x or Lodige Recycler high shear, short retention granulator, or continuous drum granulator, Eirich bread granulator or long retention, low shear granulator such as drum or cement mixer. preferable. In the case of coated agglomerates, the agglomerates prepared by known granulation methods can be used and produced in any suitable equipment such as rotary drum, pan or marmelizer type mixers.

If the agglomerates are coated with brightener particles, a binder in the coating solution (usually water) will help adhere the brightener particles to the agglomerates and form a durable bond within the coating layer. It is desirable to include.

A preferred method of forming coated agglomerates is to granulate the agglomerates with excess nonionic surfactant in a drum mixer to form "sticky" granules and then coat with brightener particles. Become. The advantage of this method is that it improves the adhesion and color of the resulting coating. It is believed that the particularly good color is due to the fact that no binder is present on the light-scattering surface of the aggregate.

A particularly preferred binder is Sokalan CP5 (manufactured by BASF), 4
It is a copolymer of maleic anhydride and polyacrylate supplied as a 0% aqueous solution.

In addition to binders, it may be necessary to use plasticizers to improve the shatter resistance of the coating. For example, the addition of 2 wt% sorbitol or glycerol to the binder spray liquor greatly reduces the friability of the agglomerates, especially when the agglomerates are air dried.

Where the agglomerates of the invention or the laundry products containing them contain a detersive activator, the latter is selected from nonionic detersive activators, anionic detersive activators, zwitterionic or amphoteric detersive activators or mixtures thereof. You can

Anionic detersive activators are water-soluble alkalis of organic sulfuric and sulfonic acids having an alkyl group containing from about 8 to about 22 carbon atoms (the term alkyl is used to include the alkyl portion of the higher acyl groups). It is usually a metal salt.
Examples of suitable synthetic anionic detergent compounds are sodium alkyl sulfate and potassium, especially e.g. premium produced from tallow or coconut oil (C ₈ ~C ₁₈₎ those obtained alcohol was sulphated, alkyl (C ₉ ~ C ₂₀ ) Sodium and potassium benzene sulphonates, especially linear secondary alkyl (C ₁₀ -C ₁₅ ) sodium benzene sulphonates; sodium alkyl glyceryl ether sulphates, especially higher alcohols and petroleum derived from tallow or coconut oil and petroleum this kind of ether synthetic alcohols derived; coconut oil fatty acid monoglyceride sodium sulfate and sulfonate; higher (C ₈ ~C ₁₈₎ fatty alcohol - alkylene oxides, especially sodium sulfate and potassium salts of ethylene oxide reaction products; coconut Esthenic acid is used for fatty acids such as fatty acids. Reaction products obtained by teruification and neutralization with sodium hydroxide; sodium and calcium salts of fatty acid amides of methyl taurine; alkane monosulfonates such as α-olefins (C ₈ -C ₂₀ ) reacted with sodium acid sulfite; Derivatives obtained by reacting paraffins with SO ₂ and Cl ₂ and then hydrolyzing with bases to form random sulfonates; and olefin sulfonates (this term refers to olefins, especially C _{10 to} C ₂₀ α-olefins. Is used for the description of the substance produced by reacting with SO ₃ and then neutralizing and hydrolyzing the reaction product). Preferred anionic detergent compounds are (C ₁₁ ~C ₁₅₎ sodium alkylbenzenesulfonate, and (C ₁₆ ~C ₁₈₎ sodium alkyl sulfate.

If the textile laundry product comprises a detergency builder material, the latter may be a material capable of reducing the amount of free calcium ions in the wash liquor, generating alkaline pH, suspending dirt removed from the textile and textile softening clay. It is preferred as it results in compositions having other advantageous properties such as dispersion of the material.

Examples of the presence of phosphorus-containing inorganic detergency builders include:
Water-soluble salts, in particular alkali metal pyrophosphates, orthophosphates, polyphosphates and sulfonates are mentioned. Specific examples of inorganic phosphate builders are the sodium and potassium salts of tripolyphosphoric acid, phosphoric acid and hexametaphosphoric acid.

When phosphorus-free inorganic detergency builders are present, examples include water-soluble alkali metal carbonates, bicarbonates, silicates and crystalline and amorphous aluminosilicates. Specific examples are sodium carbonate (with or without calcite seeds), potassium carbonate, sodium and potassium salts of bicarbonate and silicic acid.

When organic detergency builders are present, examples include alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates, polyacetylcarboxylates and polyhydroxysulfonates. Specific examples are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acid and citric acid.

Apart from the already mentioned ingredients, a number of optional ingredients may be present either as part of the clay-containing composition of the invention or as part of the overall textile laundry product.

Examples of other ingredients that may be present in the compositions of the present invention include foam boosters, foam suppressants, oxygen-releasing bleaches such as sodium perborate and sodium percarbonate, peracid bleach precursors. , Chlorine-releasing bleaches such as trichloroisocyanuric acid, inorganic salts such as sodium sulphate, and fluorescent agents, fragrances, enzymes such as proteases, liparases, cellulases and amylases, which are usually present in very small amounts, germicidal. Agents and colorants.

When the aggregate of the present invention is contained in the detergent base powder,
It is typically present at a level of 5 to 20% by weight.

A typical formulation is as follows.

Parts by weight Lauryl alkyl sulfonate 6 Nonionic detersive activator 3 Soap 1.5 Zeolite 22 Sokalan CP5 3 Alkaline silicate 0.5 Perborate monohydrate 7.5 TAED 1.8 Savinase 0.35 Carbonate 10.00 EDTA 0.15 Sulfate 24.39 SCMC 0.50 Clay aggregate 10.00 Water, Fragrances, Minor Components 9.31 Examples The present invention is illustrated by the following non-limiting examples.

Example 1A 83 parts by weight of clay (KBU, ece <50 meq / 100 g of clay, manufactured by Colin Stewart Minerals) was added to 17 parts of Synperonic A.
Clay / non-clay by spraying in a drum mixer with 3 (ICI nonionic surfactant which is a C ₁₃ -C ₁₅ alcohol ethoxylated with about 3 moles ethylene oxide per molecule and has a cloud point below 0 ° C.). An ionic surfactant aggregate was prepared.

Rotate the agglomerates in a drum coater with 20 wt% Socal U3 (SOLVAY precipitated calcium carbonate with bulk density 230 g /, particle size 4μ, R infinity 460 of 96) and 20 wt% of Sokalan CP5. Mixed. The water content of the obtained aggregate was 18%, but it was dried to a water content of 8%.

Example 1B 10 wt% Microsil (particle size 10-15μ, bulk density 130 g /
Example 1A was repeated except that the agglomerates were coated with a silica from Crosfields having a reflectance of 98.4 (R infinity 460).

Example 2 Example 1 was repeated except that the agglomerates were coated using 20 wt% Durcal (bulky density 670 g /, Omya calcite with a particle size of 4μ and a reflectance of 93 (R infinity 460)). It was

Example 3 20% by weight of Speswhite (English China Clays Ltd (EC
Example 1 was repeated except that the agglomerates were coated with kaolinite from C).

Speswhite has a bulk density of 425g /, a particle size of 80% is less than 2μ, and a reflectance of 85 (R infinity 460).

Example 4 Using 24 parts by weight of Synperonic A3 and 62 parts by weight of Sokalan CP5 2% solution as a granulation spray liquid, 83 parts by weight of clay ('KBU) was co-granulated with 83 parts by weight of Socal U3 ( co−g
ranulating) to produce clay / nonionic surfactant / precipitated calcium carbonate aggregates.

Then, the agglomerates were dried in a fluidized bed dryer using drying air at a temperature of 80 ° C. to obtain a water content of about 8%.

Example 5 Example 4 was repeated except that 83 parts by weight of Speswhite (ECC kaolin) was used instead of Socal U3 to co-granulate the agglomerates.

The reflectance of the aggregate was then measured. The numerical value of reflectance R460 ^* (infinity) shown in Table I represents the amount of light reflected from the sample and returned on a scale of 1 to 100. The higher the reflectance value, the whiter the sample. The R460 ^* value shown in the table is the least significant difference of 0.5
Is an average value of 5 times.

Table I Example R 460 ^* 1A 80 1B 80 2 58 3 66 4 80 5 62

Claims (6)

[Claims] 1. (i) A non-granulated agglomerate of a fabric softening clay and a whitening agent particle material, the co-granulated agglomerate comprising 30-60% by weight of the whitening agent particle material; and (ii) ) A coated agglomerate comprising a fabric softening clay and a whitening agent particle material, wherein the whitening agent material is present as a coating on the agglomerate of the fabric softening clay, 10-40% by weight of said A clay agglomerate selected from coated agglomerates containing particulate material, wherein the whitening agent particulate material has an average particle size of less than 20μ, a bulk density of less than 400g /, and a reflectance (R infinity 460) of more than 85. A clay aggregate characterized by being large. 2. The clay agglomerate of claim 1 having a reflectance of R infinity 460 greater than 75. 3. Agglomerate according to claim 1 or 2, wherein the whitening agent particulate material has a bulk density of less than 250 g /. 4. The aggregate according to claim 1, wherein the average particle size of the particulate material is less than 15 μm. 5. The aggregate according to claim 1, wherein the whitening agent particle material has an average particle size of less than 10 μm. 6. A detergent composition comprising 5% to 20% by weight of the agglomerate according to claim 1.