JPH0353000A - Preparation of bleaching-activating agent composition - Google Patents

Abstract

PURPOSE:To prepare the subject composition preventing the color fading of color-patterned clothes by granulating the mixed and dispersed product of a molten-soluble organic component with a bleaching-activating agent and coating the granules with a salt-sensitive water-soluble polymer. CONSTITUTION:(A) A bleaching agent-activating agent such as N,N,N',N'- tetracetylethylene diamine is mixed with (B) a molten water-soluble organic component comprising polyethylene glycol preferably having a melting point of 40-1000 deg.C or an anionic surfactant and dispersed therein, and subsequently granulated. The prepared granules are coated with a salt-sensitive water-soluble polymer preferably comprising CMC or methyl cellulose having a melting point higher than that of the component B to provide the objective composition.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a bleach activator composition. Clothes detergents containing bleaching agents have become popular in recent years because they can remove sebum stains and stains. As a bleaching agent, oxygen bleaching agents, especially percarbonates and perborates made of hydrogen peroxide adducts, are preferably used because they have no unpleasant odor and do not cause discoloration or fading on colored and patterned items. ing.

However, since these bleaching ingredients generally have a problem of poor bleaching power at low temperatures, it has been proposed to add various bleach activators to enhance the bleaching effect. Specifically, tetraacetylethylenediamine (TAED), tetraacetylglycoluril (TAGU), pentaacetylglucose (PAG), sodium nonanoyloxybenzenesulfonate (NOBS), and the like are used as bleach activators. When these bleach activators are blended into a detergent slurry and spray-dried to obtain a dry product, the bleach activators are washed away due to prolonged contact with the alkali in the slurry and high temperatures during spraying. There was a problem with it disassembling. Conventionally, therefore, a bleaching detergent composition was obtained by powder blending a bleaching agent and a bleaching activator with detergent particles. However, bleaching detergent compositions made by blending bleach activators in powder form have a problem in that the bleach activators cause local segregation due to poor macrodispersibility in the composition. Ta. Furthermore, since the bleach activator has relatively high hydrophobicity, it aggregates and floats in the bath, and there is also the problem that local segregation in the bath tends to occur. As a result, when washing with a detergent containing a bleach activator, the dyeing pigments of colored and patterned clothing often fade when colored and patterned clothing coexists, which has hindered its practical application. ．． Regarding the use of a bleach activator as a granular composition, TAED,
By granulating a stabilizer such as ethylenediaminetetraacetic acid and a nonionic surfactant, and blending the granulated product with the surfactant and sodium perborate, the storage stability of the bleaching composition can be improved. It has been reported.

Furthermore, JP-A-48-24981 describes that a bleaching aid with improved storage stability can be obtained by spray cooling a homogeneous melt consisting of a bleach activator, a fatty acid, and polyethylene glycol. It has been done. Furthermore, JP-A-47-7358 reports that storage stability can be improved by wetting a bleach activator with an aqueous liquid and mixing it with a solid coating material to form a granular composition. ing. The same publication describes aqueous solutions of cellulose derivatives such as carboxymethylcellulose as aqueous liquids, aqueous solutions or aqueous dispersions of nonionic surfactants, polyethylene glycol, etc., and carbonates as coating materials. Phosphate, silica, magnesium oxide, etc. are described.

Furthermore, bleach activators can be used such as inorganic crystalline salts, carboxymethylcellulose sodium salts, and acrylic acid copolymers. 4A
A method of granulating or mixing using type zeolite etc. (U.S. Pat. No. 3,661,741, No. 3,
Specification No. 671,439, Specification No. 3,975,280, Specification No. 3,925,234, Specification No. 4,00
No. 3,841, Specification No. 4,064,062), etc. have been reported. However, none of the bleach activators obtained by the above-mentioned conventional production methods could sufficiently prevent discoloration and fading of colored patterned objects when used in combination with a bleaching agent.

The object of the present invention is to produce a bleach activator composition that prevents discoloration and fading of colored and patterned objects. The method for producing the bleach activator composition of the present invention is as follows (A
) to (B). (A) Granulation step: A step of mixing and dispersing bleach activator powder in a molten organic water-soluble component, cooling the resulting dispersion, and granulating it. (B) Coating step 2 The granules containing the bleach activator and an organic water-soluble component obtained in step (A) above are coated with a salt-sensitive water-soluble component under a temperature condition higher than the melting point of the organic water-soluble component. The process of coating with a synthetic polymer. The present invention will be explained in more detail below. A engineer:
' First, the organic water-soluble component is heated above its melting point to melt it, and this is mixed with a powdered bleach activator and uniformly dispersed to obtain a molten mixture. This can be done using a kneading machine such as a vertical or horizontal ribbon mixer equipped with a heating device such as a jacket, or various cross-mixing machines. The melting/mixing temperature at this time can be raised above the melting point of the bleach activator, but if the temperature is too high, the bleach activator may decompose or change in quality. The water-soluble ingredients are melted and a powdered bleach activator is added to this. It is desirable to disperse. The resulting molten mixture can be pulverized into particles by crushing it with a suitable pulverizer after cooling. The obtained granulated particles are sieved as necessary to adjust the particle size. Excessive particles are crushed with appropriate equipment and sieved again.The particle size of the granulated particles containing the bleach activator and the organic water-soluble fraction is preferably about 840 to 150μ. Furthermore, the granulated product of the present invention can also be obtained by granulating the mixture of the bleach activator and the organic water-soluble component using a granulator such as a pelleter that is heated or can be heated.

(a) Organic water-soluble part and (b) bleach activator are mixed in a weight ratio of (a)/(b) = 1/4 to 6/1, preferably 173 to 1/1. It is desirable to do so. If the amount of organic water-soluble component used is too small, a large amount of fine powder will be generated after cooling and grinding, and at the same time, coating with salt-sensitive water-soluble polymer in the next process will be difficult, and the effect of preventing discoloration and fading of colored patterned objects will be reduced. to degrade. Furthermore, if the amount of bleach activator is too small, it becomes necessary to add a large amount of granules to the detergent, and this also leads to an increase in the cost of granules per unit of activator. The bleach activator is present in the final bleach activator composition in an amount of 10 to 5
It is desirable to add it so that it is blended in an amount of 0% by weight. Further, during granulation, other optional components such as carboxymethyl cellulose and sodium sulfate as dissolution control agents can also be added.

The organic water-soluble component preferably has a melting point of 40 to 100°C, more preferably 50 to 90°C. If the melting point is too low, there is a risk of melting and agglomeration during storage. On the other hand, if the melting point is too high, there is a risk that the bleach activator will decompose or change in quality during melt mixing. Preferred examples of organic water-soluble components include polyethylene glycol (preferably weight average molecular weight of 4,000 to 20,000), nonionic surfactants, and the like. Nonionic surfactants include water-soluble polyalkylene oxide adducts, for example natural or synthetic surfactants having 5 to 25 alkylene oxide units in the molecule and 8 to 22 carbon atoms in the hydrophobic part. primary or secondary alcohols, fatty acids, fatty acid amides; polyethylene oxide and/or polypropylene oxide adducts of alkylphenols; Examples include polyethylene oxide adducts of propylene glycol.

Examples of bleach activators include the following (a) to (m). Among these, (a) acylated amines, especially,
A typical example is N, N, N', N'-tetraacetylethylenediamine (TAED).

(a) N-diacylated and N,N'-tetraacylated amines, such as N,N,N',N'-tetraacetylmethylenediamine and monoethylenediamine, N,N-diacetylaniline and N,N-diacetylaniline; P-toluidine. 1.3
-Diacylated hydantoins, such as 1,3-diacetyl-5,5-dimethylhydantoin, 1,3-diprobionylhydantoin. (b) N-alkyl-N-sulfonylcarbonamides, such as N-methyl-N-mesylacetamide. N-methyl-N-mesyl-benzamide, N-methyl-N-mesyl-p-nitrobenzamide, N-methyl-N-mesyl-p-methoxybenzamide.

(c) N-acylated cyclic hydroazides, acylated triazoles or urazoles, such as monoacetylmaleic acid hydroazide.

(d) O,N,N monotrisubstituted hydroxylamines, such as O-penzoyl-N,N-succinylhydroxylamine, O-acetyl-N,N-succinylhydroxylamine, O-p-methoxybenzoyl-N,N- Succinylhydroxylamine, O-p-nitropenzoyl-N,N-succinylhydroxylamine, O,N,N-triacetylhydroxylamine. (e) N,N'-diacylsulfurylamides,
For example, N,N'-dimethyl-N,N'-diacetylsulfurylamide, N,N'-diethyl-N,N'-diprobionylsulfurylamide.

(f) Triacyl cyanurates, such as triacetyl cyanurate, tribenzoyl cyanurate.

(g) Carboxylic acid anhydrides, such as benzoic anhydride, m-chlorobenzoic anhydride, phthalic anhydride, 4-chlorophthalic anhydride.

(h) Sucrose esters, such as glycol pentaacetate. (i) 1,3-diacyl-4,5-diacyloxyimidazolidine, for example 1,3-diformyl-4,5-diacetoxyimidazolidine, 1,3-diacetyl-4,5-diacetoxy imidazolidine, 1,3-diacetyl-4. 5-dipropionyloxyimidazolidine. (j) Tetraacetyl glycoluril, tetrapropionyl glycoluril. (k) diacylated 2,5-diketopiperazine, e.g. 1,4-diacetyl-2,5
-diketopiperazine, 1,4-diprobionyl-2,5-diketopiperazine, 1,4-dipropionyl-3,G-dimethyl-2,5-diketopiperazine. (1) Propylene diurea or 2,2-dimethylpropylene diurea (2,4,6,8-tetraazabicyclo(3,3.1) monononane-3,7-dione or its 9,9-dimethyl derivative) Acylated biological compounds, especially tetraacetyl- or tetrapropionyl-propylene diurea or their dimethyl derivatives. (-)Carboxylic acid esters, such as p-(ethoxylponyloxy)-benzoic acid, p-(propoxycarbonyloxy) - Sodium salt of benzenesulfonic acid.

B. Coating A: Next, the granules obtained in step (A) are heated above the melting point of the organic water-soluble ester, and a salt-sensitive water-soluble polymer is added to coat the granules. Since the organic water-soluble component contained in the granulated particles itself partially melts and acts as a binder, there is no need to use a separate binder, and in fact, it is preferable not to use a binder. Coating can be carried out using ordinary coating equipment, stirring granulation equipment, granulation equipment, etc. The smaller the particle size of the salt-sensitive water-soluble polymer, the easier it is to coat, and it is desirable to use the salt-sensitive water-soluble polymer in an amount that accounts for 20 to 60% by weight, preferably 30 to 50% by weight of the final bleach activator composition. ．． If the amount of coating is too small, it will not be possible to sufficiently prevent discoloration and fading of colored and patterned objects, while if it is too large, the coating operation will be difficult and the effect will be saturated, which is wasteful. Examples of salt-sensitive water-soluble polymers include methylcellulose, ethylcellulose, hydroxyethylcellulose, methylhydroxypropylcellulose, carboxymethylcellulose, and methylhydroxymethylcellulose, and carboxymethylcellulose is used as a soluble salt such as sodium. Among these, carboxymethylcellulose (preferably polymerization degree iooo~3)
000), methylcellulose (preferably polymerization degree 140)
~600) is suitable. The solubility of salt-sensitive water-soluble polymers changes depending on the salt concentration, and when used in a detergent composition, the solubility of the salt-sensitive water-soluble polymer changes depending on the salt concentration.
．． 833%), the coating film is difficult to dissolve and gradually releases the bleach activator, and when cleaning with low detergent concentration (0.08%), the coating film is difficult to dissolve and gradually releases the bleach activator.
33%) is quickly dissolved and the bleach activator acts.

According to the present invention, a molten organic water-soluble component and a powdered bleach activator are mixed to obtain granulated particles, and the organic water-soluble component is mixed at a temperature higher than a certain degree of melting of the organic water-soluble component of the particles. By adding a salt-sensitive water-soluble polymer and coating the granulated particles to obtain a bleach activator composition, it is possible to prevent the color change and fading of dyeing pigments on colored and patterned items and exhibit a bleaching effect. can. Therefore, it is useful for enhancing the bleaching effect when used in combination with an oxygen-based bleach, and is particularly useful when a bleaching detergent is prepared by mixing the powder together with an oxygen-based bleach in a detergent composition.

Hereinafter, the effects of the present invention will be explained in more detail with reference to Examples, but prior to this, the evaluation method used in the Examples will be explained.

▲K blind predetermined pigment (C.I.Reactives Rad21)
Cut the dyed cloth into 7 x 7 cm pieces and fix the four corners of this dyed cloth to the frame using a bottle. Add 9g of commercial detergent that does not contain bleach to this cloth. Sprinkle with a bleach activator composition corresponding to 0.9 g of sodium percarbonate and 0.135 g of bleach activator, respectively, and further spray with water at 25 ° C.
After leaving it for 15 minutes, it is washed with water at 25°C and air-dried.

The condition of the cloth after drying was evaluated using the following criteria, and the degree of discoloration and fading was examined. 3 points: The area that came into contact with the bleaching detergent has noticeably discolored and faded, and many spots are observed. 2 points: The area that came into contact with the bleaching detergent has discolored and faded, and spots are clearly visible.

1 point: The area that came into contact with the bleaching detergent has slightly discolored and faded, and a few spots are observed.

Point O: The area that came into contact with the bleaching detergent did not change color or fade at all, and no spots were observed. Coating performance was evaluated using the following criteria based on the time required for coating using a stirring granulator. 6: Within 10 minutes 0: Within 10 to 30 minutes Δ: Within 30 to 60 minutes (Weight average molecular weight 6000
Polyethylene glycol (melting point: 60-63°C) was heated to a temperature 10-20°C higher than its melting point, and while stirring, the bleach activator shown in Table 1 and CMC as a dissolution control agent were added. (carboxymethylcellulose sodium salt, degree of polymerization 1200-1300) and sufficiently dispersed and mixed.

Then, this dispersion mixture was taken out and cooled, and 2 to 5+
After forming into a plate shape with a thickness of sm, it is coarsely crushed, further crushed in a tabletop crusher, and adjusted to a particle size of 24 to 100 mesh using a sieve. Next, the granulated particles were placed in a jacketed stirring granulation device set at a temperature higher than the melting point of the organic water-soluble component.
CMC (polymerization degree 1200-
1300) is added little by little, granulated with stirring, coated with a salt-sensitive water-soluble polymer, and then cooled to obtain a bleach activator composition. Each of these compositions was evaluated for discoloration and ease of coating, and the results are shown in Table 1 below (after Example 3). Example 2 As shown in Table 2 below, a bleach activator composition is obtained in the same manner as in Example 1 using various organic water-soluble components. For each of these compositions, discoloration and fading and particle condition after storage at 45°C were evaluated, and the results are shown in Table 2. Example 3 Bleach activator compositions were obtained in the same manner as in Example 1 using various coating agents as shown in Table 3, and discoloration and fading were evaluated and the results are shown in Table 3. (Margin below)

Claims (1)

[Claims] 1. Bleach activator powder is mixed and dispersed in the molten organic water-soluble component, this dispersion is made into particles, and the resulting particles are then processed into salt-sensitive water-soluble powder at a temperature above the melting point of the organic water-soluble component. A method for producing a bleach activator composition, which comprises coating with a polymer.