JP2005154743A - Detergent composition and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain a detergent composition capable of preventing hydrolysis of an α-sulfofatty acid alkyl ester salt and having an excellent preventing effect on solidification during storage, and to provide a method for producing the same. <P>SOLUTION: This detergent composition contains (A) particles containing 60-95 wt% of the α-sulfofatty acid alkyl ester salt in an amount of 3-40 pts.wt., (B) particles containing 5.5-25 wt% of a silicic acid salt and not substantially containing the α-sulfofatty acid alkyl ester salt in an amount of not less than 5 wt% and less than 15 wt% as the silicic acid salt, and (C) a polymer compound builder and/or a phosphoric acid salt builder in an amount of 0.1-40 wt%. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a detergent composition in which an α-sulfo fatty acid alkyl ester salt is stable and excellent in the effect of suppressing storage solidification, and a method for producing the same.

  The α-sulfo fatty acid alkyl ester salt is a surfactant having good cleaning performance. However, when a detergent composition is mixed with a slurry containing an alkaline agent (for example, carbonate or silicate) and mixed and spray-dried, a part of the slurry may be hydrolyzed. In particular, when sodium silicate is added to the slurry, the pH of the slurry is higher than that of the carbonate, so that hydrolysis is promoted.

  In recent years, a technique for producing detergent components by dry mixing without spray drying has been studied from the advantages such as low environmental load and reduction of energy cost during production. As a part of this, a technique has been proposed in which α-sulfo fatty acid alkyl ester salt is prepared as separate particles and dry-mixed with other detergent components to suppress hydrolysis during production and / or storage (Patent Document 1). : JP-A-9-169999, Patent Document 2: International Publication No. 01/90284). However, a technique for further suppressing hydrolysis has been desired.

JP-A-9-169999 International Publication No. 01/90284 Pamphlet US Pat. No. 6,509,310 US Pat. No. 6,407,050

  This invention is made | formed in view of the said situation, and it aims at providing the detergent composition which the alpha-sulfo fatty-acid alkylester salt is stable, and was excellent in the suppression effect of storage solidification property, and its manufacturing method.

  The present inventor examined the influence of each detergent component on the hydrolyzability of an α-sulfo fatty acid alkyl ester salt in a detergent process in which α-sulfo fatty acid alkyl ester salt-containing particles are dry-mixed. As a result, it was found that the decomposition of the α-sulfo fatty acid alkyl ester salt can be suppressed by incorporating a specific amount of silicate into the α-sulfo fatty acid alkyl ester salt-free particles. In addition, when the α-sulfo fatty acid alkyl ester salt particles, the silicate-containing α-sulfo fatty acid alkyl ester salt-free particles, and other components as necessary are dry-mixed, a polymer compound builder and / or phosphoric acid It was found that the solidification of the product during storage can be suppressed by adding a specific amount of salt builder. Furthermore, it has been found that the hydrolysis of the α-sulfo fatty acid alkyl ester salt is synergistically suppressed by combining this builder with the silicate-containing α-sulfo fatty acid alkyl ester salt-free particles. In the present invention, α-sulfo fatty acid alkyl ester salt-containing particles are prepared, and separately from this, silicate, which is expected to promote hydrolysis of α-sulfo fatty acid alkyl ester salt, is blended in a specific amount. -The particle | grains which do not contain a sulfo fatty-acid alkylester salt are prepared, and these obtained particles are mixed. It is a new finding by the present inventor to contribute positively to the stabilization of the α-sulfo fatty acid alkyl ester salt by doing in this way. This is presumed to occur because silicate reduces adhesion between particles and suppresses welding between detergent particles due to storage.

Accordingly, the following invention is provided.
[1]. (A) Particles containing 60-95% by mass of α-sulfo fatty acid alkyl ester salt
3-40% by mass
(B) Particles containing 5.5 to 25% by mass of silicate and substantially free of α-sulfo fatty acid alkyl ester salt
(C) High molecular compound builder and / or phosphate builder as a silicate
0.1 to 40% by mass
A detergent composition comprising:
[2]. (A) The average particle diameter of the particles is 300 to 1,200 μm, and the particle surface is coated with one or more water-insoluble inorganic powders selected from aluminosilicate and calcium carbonate. The detergent composition according to [1], which is characterized.
[3]. An average particle size of (B) particles 300~1,200μm, ₂ silicate _{Na 2 O · 2SiO, 2Na 2} O · 5SiO 2, Na 2 O · 3SiO 2, Na 2 O · 4SiO 2, ortho The detergent composition according to [1] or [2], which is one or more selected from sodium silicate, sodium sesquisilicate, and sodium metasilicate.
[4]. The polymer compound builder of component (C) is one or more selected from acrylic acid polymers, acrylic acid copolymers, polyvalent carboxylic acid polymers, and polyvalent carboxylic acid copolymers [1]. -Detergent composition in any one of [3].
[5]. (C) The detergent composition according to any one of [1] to [4], wherein the polymer compound builder content of the component is 0.8 to 10% by mass.
[6]. The detergent composition according to any one of [1] to [5], wherein the phosphate builder as the component (C) is a tripolyphosphate and / or a pyrophosphate.
[7]. The detergent composition according to any one of [1] to [6], wherein the phosphate builder content of the component (C) is 5 to 30% by mass.
[8]. The method for producing a detergent composition according to any one of [1] to [7], wherein (A) particles, (B) particles, (C) component and other components are dry-mixed.

  ADVANTAGE OF THE INVENTION According to this invention, the detergent composition which suppressed the hydrolysis of (alpha) -sulfo fatty-acid alkylester salt, and was excellent in the suppression effect of storage solidification, and its manufacturing method can be provided.

  The component (A) of the present invention is a particle containing 60 to 95% by mass of an α-sulfo fatty acid alkyl ester salt. The α-sulfo fatty acid alkyl ester salt is preferably a methyl, ethyl or propyl ester salt of a saturated or unsaturated α-sulfo fatty acid having 8 to 20 carbon atoms, and particularly a saturated or unsaturated α-sulfo fatty acid having 14 to 18 carbon atoms. The methyl ester salt is preferred.

  Components other than the α-sulfo fatty acid alkyl ester salt in the component (A) include α-sulfo fatty acid di-salt, unreacted fatty acid alkyl ester such as fatty acid methyl ester, alkyl sulfate such as sodium sulfate and methyl sulfate, excess Examples thereof include lower alcohols such as hydrogen oxide and methanol, and water. These can be used individually by 1 type or in combination of 2 or more types.

  In the particles (α-sulfo fatty acid alkyl ester salt particles), the content of particles having a particle size of 10 # (aperture 1.7 mm) or more is usually less than 2% by mass, preferably 1% by mass. Less than, more preferably less than 0.5% by mass. (A) As for the average particle diameter of particle | grains, 300-1,200 micrometers is preferable, More preferably, it is 400-700 micrometers. In addition, the measuring method of the particle average particle diameter in this invention shall be based on the method as described in an Example.

  (A) From the viewpoint of preventing sticking during the production and transportation of the particles, it is preferable to coat the surface of the (A) particles with a water-insoluble inorganic powder. Examples of the water-insoluble inorganic powder include aluminosilicates such as A-type zeolite and P-type zeolite and carbonates such as calcium carbonate. The amount of the water-insoluble inorganic powder used for the coating is preferably 5 to 30% by mass in the total amount of (A) particles. As a coating method, (A) particles and water-insoluble inorganic powder may be mixed and (A) the surface of the particles may be sufficiently coated with water-insoluble inorganic powder. As the apparatus, any mixer may be used, but a drum type mixer, a stirring granulator, a fluidized bed granulator, and the like are preferable.

As a method for producing α-sulfo fatty acid alkyl ester salt-containing particles,
(1) A method in which an α-sulfo fatty acid alkyl ester salt and an inorganic powder are dissolved in water to prepare a slurry having a water content of about 35 to 70% by mass, and this is spray-dried to obtain a dry powder.
(2) A method of obtaining particles by directly mixing an α-sulfo fatty acid alkyl ester salt paste having a water content of 20 to 30% by mass and an inorganic powder;
(3) There is a dry neutralization method in which an α-sulfo fatty acid alkyl ester and an alkaline inorganic powder are directly mixed and neutralized. Among these, the dry neutralization method (3) is preferable because it does not contain water and enables high-concentration granulation as compared with the case of using a neutralized product.

  Furthermore, in order to improve the color tone peculiar to α-sulfo fatty acid alkyl ester, a bleaching agent may be added. In addition, α-sulfo fatty acid alkyl ester and alkaline powder are mixed from the viewpoint of easily obtaining high-concentration α-sulfo fatty acid alkyl ester salt and excellent powder physical properties (fluidity and solidification suppression) during storage. A production method including a step of neutralizing and a step of aging while fluidizing the obtained mixed / neutralized powder in an apparatus equipped with an airflow generator is also preferable. As a specific method, there is a method described in JP-A-2001-64248.

  (A) Content of (alpha) -sulfo fatty-acid alkylester salt in particle | grains is 60-95 mass%, 70 mass% is preferable for a minimum, More preferably, it is 80 mass%. On the other hand, the upper limit is more preferably less than 95% by mass. When the content of α-sulfo fatty acid alkyl ester salt in the particles is too small, a large amount of particles are added when mixing the predetermined α-sulfo fatty acid alkyl ester salt, so that the merit of dry mixing is reduced. There is.

  (A) Content of particle | grains is 3-40 mass% in detergent composition, 5 mass% is preferable for the minimum of content, Preferably an upper limit is 20 mass%, More preferably, it is 15 mass%. (A) If there is too little content of particle | grains, the contribution with respect to washing | cleaning performance will decrease, and if too much, the rinsing performance after washing | cleaning may fall.

  (B) component of this invention is a particle | grain which contains 5.5-25 mass% of silicates, and does not contain (alpha) -sulfo fatty-acid alkylester salt substantially. (A) It is a particle different from the particle, and the amount of silicate is 5.5 to 25% by mass, and the particle is substantially free of α-sulfo fatty acid alkyl ester salt and is added to the detergent composition. This improves the stability of the α-sulfo fatty acid alkyl ester salt. “Substantially free of α-sulfo fatty acid alkyl ester salt” means that a small amount of α-sulfo fatty acid alkyl ester salt was unintentionally mixed in addition to the case where it does not contain α-sulfo fatty acid alkyl ester salt. Cases are also included. Specifically, when (A) particles and (B) particles are dry-mixed, (B) a fine powder of (A) particles containing α-sulfo fatty acid alkyl ester salt adheres to the surface of the particles. A case where a trace amount of an α-sulfo fatty acid alkyl ester salt is mixed unintentionally during the production process.

But it is not limited to silicate, especially, Na ₂ O · 2SiO ₂ (No. _{1), 2Na 2 O · 5SiO} 2 (2 _{No.), Na 2 O · 3SiO 2} ( No. _{3), Na 2 O · 4SiO} 2 (4 No. ), Sodium orthosilicate, sodium sesquisilicate, sodium metasilicate and the like. As these silicates, these can be used alone or in combination of two or more. From the viewpoint of usability, No. 1, No. 2, No. 3, and No. 4 silicates are preferable.

  (B) The silicate content in the particles is 5.5 to 25% by mass, the lower limit of the content is preferably 7% by mass, and the upper limit is preferably 18% by mass. If the silicate content in the particles is too high, the alkalinity of the (B) particles will increase, and the α-sulfo fatty acid alkyl ester salt will be easily hydrolyzed, and if it is too low, it will prevent adhesion between the detergent particles during storage. The effect is insufficient.

  (B) Content of particle | grains is 5 to 15 mass% as silicate in a detergent composition. The upper limit of the content is preferably 12% by mass, more preferably less than 10% by mass. In this case, the content of (B) particles is about 20% by mass or more and less than 91% by mass in the detergent composition.

  (B) Particles are various general structures disclosed in the well-known collection of conventional techniques in the field of powder detergents for clothing (see p62 to p67, items 5.1.1.1 to 5.1.3.2). Manufactured by the grain method. (B) Each component in particle | grains can add various detergent components in the range which does not impair the effect of this invention. Specifically, anionic surfactants such as linear alkylbenzene sulfonates, nonionic surfactants such as polyoxyethylene alkyl ethers, inorganic salts such as sodium carbonate, calcium carbonate and sodium sulfate, A-type zeolites and the like Add calcium scavenger, bleaching agent such as sodium percarbonate, fluorescent agent such as bis (triazinylamino) stilbene disulfonic acid derivative, bis (sulfostyryl) biphenyl salt [Tinopearl AMS-GX], [Tinopal CBS-X] You can also.

(B) The bulk density of the particles is preferably 0.3 to 1.2 g / cm ³ , and the average particle size is preferably 300 to 1,200 μm, more preferably 300 to 500 μm.

  The component (C) is a polymer compound builder and / or a phosphate builder. (C) By mix | blending a component, the solidification suppression effect of a composition can be provided.

  Examples of the polymer compound builder include acrylic acid polymer and copolymer, polycarboxylic acid polymer and copolymer, and specifically, polyacrylic acid, acrylic acid-allyl alcohol copolymer, acrylic acid. -Maleic acid copolymer, polysaccharide-acrylic acid copolymer, hydroxyacrylic acid copolymer, those obtained by polymerizing or copolymerizing monomers such as maleic acid, itaconic acid, fumaric acid, etc., and salts thereof. Of these, acrylic acid maleic acid copolymer, polyacrylic acid and salts thereof are preferred.

  Examples of the phosphate builder include tripolyphosphate and pyrophosphate, among which sodium tripolyphosphate is preferable. As the component (C), a polymer compound builder and a phosphate builder can be used singly or in appropriate combination of two or more.

  (C) Content of a component is 0.1-40 mass% in detergent composition. When blending a polymer compound builder, the lower limit of the content is preferably 0.8% by mass, more preferably 1.0% by mass, and even more preferably 1.5% by mass. An upper limit becomes like this. Preferably it is 15 mass%, More preferably, it is 10 mass%, More preferably, it is 8 mass%. When blending a phosphate builder, the lower limit of the content is preferably 5% by mass, more preferably 10% by mass, and the upper limit is preferably 30% by mass, more preferably 20% by mass.

  (C) A component may be mix | blended separately from (A) particle | grains and (B) particle | grains, and may be mix | blended in (A) particle | grains and (B) particle | grains. In particular, it is preferable to blend in the (B) particles.

  In the detergent composition of the present invention, in addition to the above essential components, other components such as various additives for improving performance and functions can be blended within a range not impairing the object of the present invention. Specifically, inorganic salts such as sodium carbonate, calcium carbonate and sodium sulfate, calcium scavengers such as A-type zeolite, bleaching agents such as sodium percarbonate, bis (triazinylamino) stilbene disulfonic acid derivatives, bis (sulfo Styryl) biphenyl salt [Tinopearl AMS-GX], [Tinopearl CBS-X] and other fluorescent agents, linear alkylbenzene sulfonate, alkyl sulfate, α-olefin sulfonic acid, polyoxyethylene alkyl ether sulfate, secondary alkane Examples include sulfonates, soaps, polyoxyethylene alkyl ethers, surfactants such as alcohol EO / PO adducts, bleaching activators, characteristic imparting components such as enzyme particles, fragrances, dyes, pigments and the like. When these optional components are blended in the detergent composition, they may be blended separately from (A) particles and (B) particles, or may be blended in (A) particles and (B) particles.

  The detergent composition of the present invention can be obtained by mixing (preferably dry-mixing) the (A) particles, (B) particles, (C) component obtained by the above method and other components as required. Here, dry mixing is generally a method of producing by simply blending a powder raw material and a small amount of liquid raw material.

Any mixer can be used as long as various particles can be sufficiently mixed with each other, but a horizontal cylindrical type, a double cone type, a V type, a rotation / revolution type, etc. Can be suitably used. Moreover, you may use a stirring granulator and a rolling granulator. Preferably, a horizontal cylindrical type, a double circular lead type, a V type, a rotation / revolution type, or the like is used, and the temperature is 10 to 50 ° C., the Fr number is 0.01 to 0.6, preferably 0.1 to 0 .5 (Fr = V ² / (R × g), V: peripheral speed (m / s) at the tip of the stirring blade, R: rotation radius (m) of the stirring blade, g: acceleration of gravity (m / s ² ) ). At this time, the order of addition of various particles and other components is not particularly limited, but it is preferable to add a granulated product such as an enzyme or a bleaching agent at the final stage in order to avoid destruction of the granulated product.

  EXAMPLES Hereinafter, although a preparation example, an Example, and a comparative example are shown and this invention is demonstrated concretely, this invention is not restrict | limited to the following Example. In the following examples, unless otherwise specified, “%” in the composition represents mass%.

[Preparation Examples (A) 1-3]
(A) Preparation of α-sulfo fatty acid alkyl ester salt (hereinafter referred to as MES) particles (hereinafter referred to as MES particles) α-sulfo fatty acid alkyl ester salt particles having the composition shown in Table 1 were obtained by the following production method. The particle size distribution of the particles was measured based on the JIS sieve method, and the average particle size was measured based on the following method.

Measuring method of average particle diameter For each sample and a mixture thereof, a 9-stage sieve and a saucer having openings of 1,700 μm, 1,400 μm, 1,180 μm, 1,000 μm, 710 μm, 500 μm, 300 μm, 250 μm, and 180 μm are used. The classification operation was performed. In the classification operation, a sieve with a small opening is stacked on a tray in the order of a sieve with a large opening, and a sample of 100 g / time is placed on the top of the top 1,700 μm sieve. (Made by Iida Seisakusho Co., Ltd., tapping: 156 times / minute, rolling: 290 times / minute) After shaking for 10 minutes, the sample remaining on each sieve and the saucer was collected for each sieve, The mass of the sample was measured.
When the mass frequency of the tray and each sieve is integrated, the opening of the first sieve where the integrated mass frequency is 50% or more is set to a μm, and the opening of the sieve that is one step larger than a μm is set to b μm. The average particle size (weight: 50%) was calculated by the following equation, where c% was the cumulative mass frequency from the sieve to the aμm sieve and d% was the mass frequency on the aμm sieve.

(1) Preparation of α-sulfo fatty acid alkyl ester salt-containing paste (sulfonation step)
Sulfonation was performed in the reaction tank 1 shown in FIG.
The apparatus was made of SUS316L with a capacity of 200 L, jacket cooling, and a stirrer 3 and the reaction temperature was controlled by a circulation line 7. First, 80 kg of raw fatty acid methyl ester was charged into the reaction vessel 1, and 5% of finely powdered sodium sulfate was added to the fatty acid methyl ester as a coloring inhibitor while stirring well. While continuing stirring, the reaction temperature was 80 ° C., the circulation amount in the circulation line 7 was 80 L / min, and SO ₃ gas (sulfonated gas) diluted to 8% by volume with nitrogen gas was 102 m ³ (1 relative to the raw material methyl ester). .2 mol) was blown from the ring sparger of the gas introduction pipe 5 at a constant speed over 1 hour. Further, aging was performed for 30 minutes while maintaining at 80 ° C.

(Esterification process)
As the esterification reaction tank 10, a jacketed three-stage stirring tank type was used. Further, as the lower alcohol, methanol was supplied at 4.5 kg / hr (hour), and the esterification was carried out by controlling to 4% by mass with respect to the sulfonated product. The reaction rate of esterification was 80 ° C. and the time was 30 minutes.

(Neutralization process)
Subsequently, the sulfonated product extracted from the esterification reaction tank 10 was continuously supplied to the neutralization line 17 at 117 kg / hr. The neutralization method employs the neutralization method described in JP-A No. 2001-64248. Between the premixer 14 and the neutralization mixer 15, a 35 mass% sodium hydroxide aqueous solution is fed at a rate of 46.6 kg / hr. Was fed quantitatively and continuously neutralized. The sulfonated product was previously mixed with the pre-neutralized product with the premixer 14 in advance, and then mixed with an aqueous sodium hydroxide solution to obtain a neutralized product. The amount of the pre-neutralized product circulating through the loop was 20 times the total amount of the sulfonated product and the alkaline aqueous solution to be added. The neutralization temperature was controlled at 70 ° C. by adjusting the water temperature in the heat exchanger 16 of the loop circuit. The residence time of the neutralized product was 20 minutes. Although not shown in FIG. 1, a pH control system is installed in the circulation loop, and the supply rate (supply amount) of the sodium hydroxide aqueous solution is controlled by a Ford back controller that adjusts the supply rate of the sodium hydroxide aqueous solution. Controlled. The pressure inside the circulation loop was 4 kg / cm ² . The pH of the obtained neutralized product was 6.5.

(Bleaching process)
Subsequently, this neutralized product was fed to the bleaching agent mixing line 21 at a feed rate of 164 kg / hr. The bleaching agent mixing line 21 was a circulation loop system including a circulation line 22 having a heat exchanger 20. Then, 35% hydrogen peroxide solution was supplied at a pure content of 1.0% to 6.6 kg / hr (AI: α-sulfo fatty acid alkyl ester salt), and neutralized after bleaching from the circulation line 22 Thoroughly mixed with the product (pre-bleached). The amount of loop circulation was 15 times the amount of neutralized product newly added to the preliminary bleached product, and the pressure in the circulation loop pipe was 4 kg / cm ² . The temperature of the circulation loop was adjusted to 80 ° C. by the heat exchanger 20, and the residence time of the circulation loop was 10 minutes. Subsequently, it was introduced into a distribution pipe type bleaching line 23 to proceed with bleaching. The bleaching line 23 is a jacketed double tube, and the temperature and pressure can be adjusted. The flow of the bleaching agent mixture was a piston flow, the pressure was adjusted to 4 kg / cm ² , the temperature was adjusted to 80 ° C., and the residence time was 180 minutes.

(2) First aging step Next, the composition after the bleaching step was transferred to the bleach tank 25 and aged in 3 to 24 hours while maintaining the temperature at 60 to 90 ° C to obtain an α-sulfo fatty acid alkyl ester salt-containing paste. .

(3) Preparation of α-sulfo fatty acid alkyl ester salt-containing particles (concentration step)
Vacuum thin film evaporator Exeva (heat transfer surface: 0.5 m ² , inner diameter: Rotating the α-sulfo fatty acid alkyl ester salt-containing paste obtained above at a rotation speed of 1,060 rpm and a blade tip speed of about 11 m / sec. 205 mm, clearance between heat transfer surface and blade tip: 2 to 4 mm, manufactured by Shinko Pantech Co., Ltd.) at 50 to 90 kg / hr, inner wall heating temperature 120 to 140 ° C., vacuum degree 0.007 to 0.00. Concentration was performed at 014 MPa to obtain α-sulfo fatty acid alkyl ester salt-containing particles. The temperature of the obtained particles was 70 to 90 ° C.

(4) Coating The particles prepared in the above (3) were subsequently introduced into a drum mixer and coated with the amount of A-type zeolite shown in Table 1 for the particles A2 and A3 in Table 1.

[Preparation Examples (B) 1-4]
(B) Preparation of particles containing silicate and substantially free of α-sulfo fatty acid alkyl ester salt (hereinafter referred to as silicate-containing MES non-containing particles) A 70 ° C. aqueous detergent slurry was prepared. The order of adding the raw materials was not particularly limited. After the final component was added, the slurry was mixed at 70 ° C. for about 2 hours, and dried using a countercurrent spray drying tower at a hot air temperature of 260 ° C. to a moisture content of about 6% to obtain a spray-dried powder.

[Examples 1 to 9, Comparative Examples 1 and 2]
After (A) MES particles, (B) silicate-containing MES-free particles, (C) component and optional components are dry (powder) mixed, the entire detergent composition is coated with zeolite, and finally a fragrance is sprayed. Detergent compositions having the compositions shown in Tables 3 and 4 were obtained. The storage stability and solidification suppression of the obtained detergent composition were evaluated by the following methods. The results are also shown in Tables 3 and 4.

[Comparative Example 3]
MES particles A1 were added to the slurry for B1 particles so as to have the same composition as in Example 1, stirred at 70 ° C. for 2 hours, and then spray-dried. Evaluation was performed in the same manner as in the examples.

Evaluation and measurement methods are shown below.
Storage stability Storage method: Put 500 g of the detergent composition in a polyethylene gusseted container for filling 500 g, and cycle for 45 ° C, 16 hours, relative humidity 85%, 25 ° C, 8 hours, relative humidity 65% (1 day) ) And stored for 1 month to prepare a storage stability test sample.

The di-Na (α-sulfo fatty acid disodium salt (hydrolyzed product) production rate% of the detergent composition after the storage was measured.
Under the following HPLC measurement conditions, the amount of di-Na produced after storage (peak area) and the amount of di-Na (peak area) when MES in the detergent composition was forcibly hydrolyzed (high temperature / alkaline conditions) ) Was measured. From the obtained amount of di-Na (peak area), di-Na production rate% (di-Na produced after the above storage relative to the amount of di-Na when MES in the detergent composition is forcibly hydrolyzed 100%) -Ratio of Na amount (% by mass)) was calculated.
(HPLC measurement conditions)
Column: NUCLEOSIL 100-5SB (GL inner diameter 4.6 mm, column length 150 mm) manufactured by GL Science Co., Ltd. (GL Science)
RI detector: manufactured by GL Science, model 504 (solvent used: sodium perchlorate 0.7%, methanol / ion-exchanged water = 80/20 (volume ratio), column temperature: 40 ° C.)

Solidification The above detergent composition after storage is taken out on a 4 # (4 mm mesh) sieve, and the mass (A) g of the detergent remaining on the sieve and the mass (B) g of the detergent that has passed through the sieve are obtained. The solidification rate (%) was calculated based on the following formula.
Solidification rate (%) = [A / (A + B)] × 100 (%)

＊上記比較例３の調製方法で調製した。実施例２と同組成である。

* Prepared by the preparation method of Comparative Example 3 above. The composition is the same as in Example 2.

  From the results of Comparative Example 3, it was found that when MES was blended in (B) particles, the di-Na production rate (%) after storage was high.

The raw materials used in the preparation examples, examples and comparative examples are shown below.
MES: Sodium salt of α-sulfo fatty acid methyl ester A fatty acid methyl ester (C ₁₆ / C ₁₈ ratio = 45/55) obtained by transesterification of palm oil with methanol was converted into sulfone according to the above-described method for preparing MES paste. Obtained. About 66% pure
α-sulfo fatty acid alkyl ester sodium pure 66%
-Sodium silicate: JIS No. 1 sodium silicate (manufactured by Nippon Chemical Industry Co., Ltd.), pure content of about 44% (solid content)
Acrylic acid maleic acid copolymer: sodium salt of acrylic acid-maleic acid copolymer, trade name Socaran CP7 (manufactured by BASF), about 40% pure (solid content)
LAS-Na: linear alkylbenzene sulfonic acid sodium salt By neutralizing the linear alkylbenzene sulfonic acid of Alkene L (pure content: about 96%) manufactured by Nisseki Detergent Co., Ltd. with a 48% aqueous sodium hydroxide solution. Use the prepared one Soap: Fatty acid sodium having 12 to 18 carbon atoms (manufactured by Lion Corporation, pure content: 67%, titer: 40 to 45 ° C., fatty acid composition: C ₁₂ : 11.7%, C ₁₄ : 0.4%, C ₁₆ : 29.2%, C ₁₈ (stearin): 0.7%, C ₁₈ (olein): 56.8%, C ₁₈ (linol): 1.2%, molecular weight: 289) , 67% pure
-AOS-Na: α-olefin sulfonic acid sodium salt α-olefin sulfonic acid sodium salt having an alkyl group having 14 to 18 carbon atoms, pure content 55%
In addition, about what was described above, the compounding quantity converted into the pure part is shown in a table | surface.

The blending amounts in the table for those listed below are not converted into pure components, but represent the blending amounts of the products blended below.
-Type A zeolite: (Mizusawa Chemical Co., Ltd., Shilton B) containing about 20% water in the powder-Tripolyphosphate: Mitsui Chemicals Co., Ltd., trade name: Tripolyphosphate soda (manufactured by Lion Co., Ltd.) Aqueous slurry with 55% pure content)
・ Sodium carbonate: manufactured by Asahi Glass Co., Ltd., granular ash ・ Calcium carbonate: manufactured by Nitto Flour Chemical Co., Ltd. ・ Sodium sulfate: manufactured by Shikoku Kasei Kogyo Co., Ltd., neutral anhydrous sodium sulfate K
・ Fluorescent agent CBS: Chino Pearl CBS-X (manufactured by Ciba Specialty Chemicals)
・ Fluorescent agent AMS: Chino Pearl AMS-GX (manufactured by Ciba Specialty Chemicals)
Enzyme: Novozyme, Sabinase 12T
Fragrance: Fragrance composition A described in JP-A No. 2002-146399

It is the schematic block diagram which showed an example of the apparatus used for the manufacturing method of the particle | grains containing 60-95 mass% of (A) alpha-sulfo fatty-acid alkylester salt of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Reaction tank 2 Raw material liquid phase 3 Stirrer 4 Sulfonation gas introduction port 5 Gas introduction pipe 6 Exhaust gas port 8 Feed pump 7 Sulfonation external circulation line 9 Sulfonation external circulation heat exchanger 10 Esterification reaction tank 11 Esterification buffer tank DESCRIPTION OF SYMBOLS 12 Esterification acid supply pump 13 Neutralization recycle pump 14 Neutralization premixer 15 Neutralization mixer 16 Neutralization heat exchanger 17 Neutralization line 18 Bleaching mixer 19 Bleaching recycle pump 20 Bleaching heat exchanger 21 Bleaching agent mixing line 22 Bleach circulation Line 23 Bleaching line 24 Vacuum deaerator 25 Bleaching tank

Claims (8)

(A) Particles containing 60-95% by mass of α-sulfo fatty acid alkyl ester salt
3-40% by mass
(B) Particles containing 5.5 to 25% by mass of silicate and substantially free of α-sulfo fatty acid alkyl ester salt
(C) High molecular compound builder and / or phosphate builder as a silicate
0.1 to 40% by mass
A detergent composition comprising:   (A) The average particle diameter of the particles is 300 to 1,200 μm, and the particle surface is coated with one or more water-insoluble inorganic powders selected from aluminosilicate and calcium carbonate. A detergent composition according to claim 1 characterized in that An average particle size of (B) particles 300~1,200μm, ₂ silicate _{Na 2 O · 2SiO, 2Na 2} O · 5SiO 2, Na 2 O · 3SiO 2, Na 2 O · 4SiO 2, ortho The detergent composition according to claim 1 or 2, wherein the detergent composition is one or more selected from sodium silicate, sodium sesquisilicate, and sodium metasilicate.   2. The polymer compound builder of component (C) is one or more selected from acrylic acid polymers, acrylic acid copolymers, polyvalent carboxylic acid polymers, and polyvalent carboxylic acid copolymers. The detergent composition according to any one of -3.   The detergent composition according to any one of claims 1 to 4, wherein the polymer compound builder content of the component (C) is 0.8 to 10% by mass.   The detergent composition according to any one of claims 1 to 5, wherein the phosphate builder (C) is a tripolyphosphate and / or a pyrophosphate.   The detergent composition according to any one of claims 1 to 6, wherein the phosphate builder content of the component (C) is 5 to 30% by mass.   The method for producing a detergent composition according to any one of claims 1 to 7, wherein (A) particles, (B) particles, (C) component and other components are dry-mixed.

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