WO2004035717A1 - PARTICLE CONTAINING α-SULFOFATTY ACID ALKYL ESTER SALT, PROCESS FOR PRODUCING THE SAME, AND DETERGENT - Google Patents

Abstract

A process for producing particles containing an α-sulfofatty acid alkyl ester salt, characterized by comprising the step of mixing an α-sulfofatty acid alkyl ester with an alkaline powder to neutralize the ingredients and the step of aging the resultant mixed and neutralized powder while fluidizing it in an apparatus equipped with a stream generator. Thus, an α-sulfofatty acid alkyl ester salt having a high concentration can be easily obtained. Particles containing a high-concentration α-sulfofatty acid alkyl ester salt can also be obtained which are excellent in powder properties during storage (flowability and unsusceptibility to caking).

Description

TECHNICAL FIELD The present invention relates to monosulfo fatty acid alkyl ester salt-containing particles, a method for producing the same, and a detergent.

 The present invention relates to high-concentration monosulfofatty acid alkyl ester salt-containing particles having improved powder properties during storage, a method for producing the same, a detergent containing the α_sulfofatty acid alkyl ester-containing particles, and a detergent comprising the same. Pertains to a filled detergent product. Background art

 There are two typical methods for producing the monosulfo fatty acid alkyl ester salt-containing particles. One is a method in which a sulfo fatty acid alkyl ester salt and 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. . The other is a method of directly mixing an α-sulfofatty acid alkyl ester salt paste having a water content of 20 to 30% by mass with an inorganic powder to obtain particles.

 In the former, drying is performed, so that relatively high concentration of particles containing a monosulfofatty acid alkyl ester salt can be produced. However, it uses a very large amount of energy and emits exhaust gas into the atmosphere, so there is a great concern about the burden on the environment. In addition, hydrolysis is a problem because it passes through a slurry with a high water content. As a result, their use has been decreasing in recent years.

 On the other hand, in the latter method, both the energy consumption and the environmental load are smaller than in the former method. However, due to the large amount of water contained in the sulfosulfate fatty acid alkyl ester salt, if the content ratio is high, the physical properties of the mixture become close to a paste, and granulation becomes extremely difficult. In addition, when water is contained, hydrolysis becomes a problem as in the spray drying method. As an improvement method, it is possible to concentrate the paste to a water content of 10% by mass or less, solidify it by cooling, and pulverize the paste to obtain particles, but the process becomes complicated and the solubility of the obtained particles is increased. Is a very big problem.

As a method for solving these problems and realizing higher concentration, there are α-sulfofatty acid alkyl esters and α-sulfofatty acid alkyl esters which can be handled without containing water. There is a dry neutralization method for directly mixing and neutralizing a lukalic inorganic powder. Since this method does not contain water, high-concentration granulation is possible as compared with the case where a neutralized product is used. This technique of dry neutralization has been known for a long time, and in particular, dry neutralization using LAS (linear alkylbenzene sulfonic acid) is widely used. Although there are few examples of α-sulfofatty acid alkyl esters, Japanese Patent Application Laid-Open (JP-A) Nos. 61-87765, 62-298570, It is described in Japanese Unexamined Patent Publication No. Hei 6—5202665. These are obtained by mixing an α-sulfofatty acid alkyl ester and an alkaline inorganic powder such as sodium carbonate to obtain a neutralized product, and the obtained neutralized product is pulverized and granulated. In some cases, a bleaching agent may be added to improve the color tone specific to α-sulfofatty acid alkyl esters.

 However, these methods cause problems such as solidification or deterioration of fluidity when the obtained particles containing the monosulfo fatty acid alkyl ester salt are stored. From the above, high-concentration α-sulfofatty acid alkyl ester salt-containing particles that can easily obtain a high-concentration alkyl sulfofatty acid salt and have excellent powder properties (fluidity and solidification) during storage Was desired. Disclosure of the invention

 The present invention relates to a high-concentration α-sulfofatty acid alkyl ester salt-containing particle which suppresses hydrolysis and is excellent in powder properties (flowability and solidification) during storage; It is an object of the present invention to provide a production method which can be easily obtained, a detergent containing the particles containing the high-concentration α-sulfo fatty acid alkyl ester salt, and a detergent product filled with the particles containing the α-sulfo fatty acid alkyl ester salt and the detergent. The purpose is.

 The present inventors have prepared a powder obtained by mixing an α-sulfofatty acid alkyl ester and an alkaline powder when producing particles containing an α-sulfofatty acid alkyl ester salt, The inventors have found that the above object can be achieved by aging while fluidizing in a device equipped with a generator, and have accomplished the present invention.

Specifically, α-sulfofatty acid alkyl ester salt produced by dry neutralization The problems with the contained particles are that the powder properties (fluidity, solidification) deteriorate immediately after production and during storage. The causes are the neutralization rate and the characteristic of alkyl sulfonate. Crystallization speed (crystal stabilization speed). Generally, dry neutralization is slower than neutralization in liquid. In the case of monosulfo fatty acid alkyl ester salt, this phenomenon is considered to be remarkable, and it is extremely high compared to other activators such as linear alkyl benzene sulfonate (LAS salt) and alkyl sulfate (AS salt). Slow. Therefore, after mixing with the alkali powder, the particles gradually become neutralized after being granulated, and the temperature rises due to the heat of neutralization generated at that time. It is considered that this phenomenon and the slowness of the crystal acceleration cause solidification and deterioration of fluidity during storage. On the other hand, hydrolysis is carried out by preparing a powder in which a monosulfo fatty acid alkyl ester and an alkaline powder are mixed, and then aging the mixed powder while fluidizing it in a device equipped with an airflow generator. Thus, high-concentration α-sulfofatty acid alkyl ester salt-containing particles having excellent powder physical properties (fluidity and solidification) during storage can be obtained.

 Accordingly, the present invention provides the following method for producing α-sulfofatty acid alkyl ester salt-containing particles, monosulfo fatty acid alkyl ester salt-containing particles, a detergent, and a detergent product.

 (1) A step of mixing and neutralizing an α-sulfofatty acid alkyl ester and an alkaline powder, and a step of ripening the obtained mixed and neutralized powder while fluidizing it in an apparatus equipped with an air flow generator. A method for producing particles containing α-sulfofatty acid alkyl ester salt, comprising:

 (2) The method further includes a step of bleaching the α-sulfofatty acid alkyl ester and / or the monosulfofatty acid alkyl ester salt with hydrogen peroxide or a compound generating hydrogen peroxide. The manufacturing method as described.

 (3) The method according to (1) or (2), wherein the step of mixing and neutralizing the α-sulfofatty acid alkyl ester and the alkaline powder is performed in a fluidized bed.

(4) α-sulfofatty acid alkyl obtained by contacting a fatty acid alkyl ester with a sulfonating gas in the presence of a coloring inhibitor to form a sulfonated fatty acid alkyl ester, and esterifying the obtained sulfonated product with a lower alcohol S The production method according to any one of (1) to (3), which is a tellurium.

(5) An α-sulfofatty acid alkyl ester salt-containing particle produced by the production method according to any one of (1) to (4) and containing 7 to 80% by mass of an α-sulfofatty acid alkyl ester salt.

 (6) A detergent comprising the monosulfofatty acid alkyl ester salt-containing particles according to (5).

(7) A detergent product in which the particles containing the sulfosulfo fatty acid alkyl ester salt according to (5) or the detergent according to (6) is filled in a packaging container made of paper, plastic, or a composite material of paper and plastic. . BEST MODE FOR CARRYING OUT THE INVENTION

 The first invention is a process of mixing and neutralizing the alkyl sulfonate and the alkaline powder, and aging while mixing and neutralizing the obtained mixed and neutralized powder in a device equipped with an airflow generator. And .alpha.-sulfofatty acid alkyl ester salt-containing particles obtained by the method. The α-sulfofatty acid alkyl ester salt-containing particles include, as described later, an α-sulfofatty acid alkyl ester and / or a sulfofatty acid alkylester salt, an alkaline powder, and, if necessary, a monosulfofatty acid alkylester. Contains bleaching agents for bleaching, surface modifiers such as zeolite, and pigments.

 The first step of the method for producing the monosulfofatty acid alkyl ester salt-containing particles of the present invention is a step of mixing and neutralizing the α-sulfofatty acid alkyl ester and the alkaline powder.

 The α-sulfofatty acid alkyl ester is an acid precursor, and is neutralized into a sulfosulfofatty acid alkyl ester salt by mixing with an alkaline powder described later. In this case, the α-sulfofatty acid alkyl ester and the α-sulfofatty acid alkyl ester salt are represented by the following formulas (1) and (2), respectively.

R ^ CH-COR ² Ri-CH-COR ²

 I (1) '' I (2)

SO, H S0 ₃ M (In the formula, R ′ is a saturated or unsaturated monovalent hydrocarbon group having 6 to 24 carbon atoms, particularly 10 to ²⁰ carbon atoms, and R ² is a linear or branched alkyl group having 1 to 6 carbon atoms. , Preferably a methyl group, an ethyl group, or a propyl group, and M represents Na or K.)

 The alkyl sulfosulfate fatty acid of the present invention can be obtained according to a conventional method or a method described in JP-A-2001-64248. In particular, α-sulfo fatty acid alkyl esters obtained by contacting a fatty acid alkyl ester with a sulfonating gas in the presence of a coloring inhibitor and sulfonating the obtained sulfonated product with a lower alcohol and then esterifying the sulfonated product are preferred. As the coloring inhibitor, sodium sulfate and potassium sulfate are preferable, and as the lower alcohol, it is preferable to use methanol, ethanol, or a mixture thereof. By using the α-sulfofatty acid alkyl ester produced by this method, it is possible to obtain α-sulfofatty acid alkyl ester salt-containing particles with suppressed coloring.

 Examples of the alkaline powder include, but are not particularly limited to, alkali metal carbonates, alkali metal silicates, and alkali metal phosphates. Examples of the alkali metal carbonate include sodium carbonate, potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, and sodium potassium carbonate.Examples of the alkali metal silicate include sodium silicate and layered sodium silicate. Examples of the alkali metal phosphate include sodium tripolyphosphate and sodium pyrophosphate. Of these, alkali metal carbonates are preferable, and among them, sodium carbonate, potassium carbonate, and sodium potassium potassium carbonate are particularly preferable. One or more of these can be used.

 The particle size of the alkaline powder is from 0.1 to 500 m as an average particle size, preferably from 0.2 to 400 m, particularly preferably from 0.5 to 300 m, more preferably from 0.7 to 500 m. 200 m.

The mixing ratio of the sulfo fatty acid alkyl ester and the alkaline powder is preferably α-sulfo fatty acid alkyl ester: alkaline powder (molar ratio) = 1: 0.85 to 1:12, particularly 1: 0.85-1: 11 is preferred. If the molar ratio of the alkaline powder to α-sulfofatty acid alkyl ester 1 is less than 0.85, neutralization is promoted, and degassing of carbon dioxide generated during the reaction may not be performed smoothly. . on the other hand, If it exceeds 12, the effect does not change, but the concentration of monosulfofatty acid alkyl ester may inevitably decrease.

 The conditions for mixing and neutralizing the α-sulfofatty acid alkyl ester and the alkaline powder are not particularly limited. As a general mixing method, a raw material powder containing an alkaline powder is charged into a mixing apparatus. Then, a method of adding a monosulfofatty acid alkyl ester is used. The temperature of the α-sulfofatty acid alkyl ester at the time of addition is preferably 30 to 90 ° C. The addition of the alkyl sulfosulfate is preferably carried out by spraying or dropping. The fluidized state of the powder at the time of addition is not limited. Since the temperature of the granulated product during mixing rises due to the generated heat of neutralization, the temperature may exceed 100 ° C in an apparatus without a heat removal mechanism. And α-sulfofatty acid alkyl ester salt-containing particles free of the above.

 The mixing device is not particularly limited as long as it is a device having a structure capable of mixing the α_sulfofatty acid alkyl ester and the inorganic powder, but examples thereof include a fluidized bed device and a stirring granulator.

 The fluidized bed device is provided with an airflow generator, and is a device that fluidizes the powder by the airflow. Examples of the fluidized bed device are G1 att—POWR EX series [manufactured by Parex Corporation] and MIXGRAD series [Okawara Corporation] Manufacture].

 The stirring granulation device is a device having a stirring blade and a stirring shaft at the center of the inside. Examples thereof include a Henschel mixer [manufactured by Mitsui Miike Kakoki Co., Ltd.] and a high speed mixer [Fukae Kogyo Co., Ltd.] Co., Ltd.], Vertical Granule Yule One-Yuichi [Palek Co., Ltd.], Redige Mixer [Matsubo Co., Ltd.], and Pro-Share Mixer [Pacific Machine Co., Ltd.].

 As the mixing device used in the present invention, a fluidized bed device is preferable. This is because the fluidized bed apparatus granulates while sending air, so that the heat of neutralization generated during mixing is removed, the temperature of the granulated material can be kept low, and high concentrations of α-sulfo fatty acid alkyl This is because the production of the ester salt-containing particles becomes possible.

The case where the first step is performed in a fluidized bed (fluidized bed apparatus) will be described below. First, a powder containing an alkaline powder is charged into a fluidized bed. At this time, the average thickness of the powder layer during standing is preferably about 50 to 500 mm. After that, air is blown into the fluidized bed, After fluidizing, spraying of α-sulfofatty acid alkyl ester is started. The spraying of the α-sulfofatty acid alkyl ester preferably uses a two-fluid nozzle in order to improve atomization. The average droplet diameter at this time is preferably about 5 to 500. As the spraying proceeds, the granulation progresses and the particle size increases, so granulation is performed while adjusting the wind speed to maintain a fluidized state. The wind speed is adjusted in the range of 0.2 to 4. O m / s, and the wind temperature is adjusted to 5 to 70 ° C, preferably 7 to 65. It is preferable to perform the production while periodically dropping the fine particles adhering to the bag filter with pulsed air.

 In order to promote the neutralization, a small amount of a liquid containing water may be added after spraying the α-sulfofatty acid alkyl ester. The liquid is preferably water or an alkaline aqueous solution in which a water-soluble alkali metal is dissolved. When the particle temperature after aging is high, it is preferable to cool by switching the air to cool air.

 The second step of the method for producing the α-sulfofatty acid alkyl ester salt-containing particles of the present invention is a step of ripening the obtained mixed / neutralized powder while fluidizing it in an apparatus equipped with an airflow generator. It is.

 Here, the term “aging” refers to holding at a predetermined temperature for a predetermined time. The aging can prevent the obtained α-sulfofatty acid alkyl ester salt-containing particles from solidifying during storage and from deteriorating the fluidity of the particles. The aging temperature is preferably from 5 to 130 ° C, particularly preferably from 10 to 120 ° C. If the aging temperature is lower than 5 ° C, neutralization and crystallization may not proceed. On the other hand, if the temperature exceeds 130 ° C., fluidization may not occur due to deterioration of physical properties. The fluidization time is at least 30 seconds, especially at least 60 seconds, more preferably at least 120 seconds, most preferably at least 300 seconds. If the fluidization time is less than 30 seconds, neutralization and crystallization are not sufficient, and powder physical properties may deteriorate during storage. The upper limit of the aging time is not particularly limited, but is usually about 1 hour.

The apparatus used in the aging step is an apparatus equipped with an airflow generator, and is not particularly limited as long as the apparatus is capable of introducing an airflow and fluidizing particles. Preferably, a fluidized bed apparatus and a stirring granulation apparatus capable of introducing a gas stream are used. The gas used for the airflow includes air. The mixing / neutralizing step and the aging step can be performed in the same apparatus. When the mixing / neutralization step and the aging step are performed in the same fluidized bed, the air is continuously sent even after spraying the α-sulfo fatty acid alkyl ester, and the fluidized state is maintained.

 Further, it is preferable to include a step of bleaching the alkyl sulfonate and / or the alkyl ester of α-sulfo fatty acid with hydrogen peroxide or a compound generating hydrogen peroxide. This step may be performed at the same time as the step of mixing and neutralizing the alkyl sulfo fatty acid ester and the alkaline powder or the step of aging the obtained mixed and neutralized powder. It may be performed before, after the mixing and neutralization steps, before the aging step, or after the aging step. By adding a bleaching agent such as an aqueous hydrogen peroxide solution, bleaching and neutralization can be promoted simultaneously. The step of bleaching the alkyl sulfo fatty acid ester and / or the alkyl ester of α-sulfofatty acid includes the step of mixing and neutralizing the alkyl powder of α-sulfofatty acid and the alkaline powder; A step of aging the neutralized powder, before the mixing / neutralization step, after the mixing / neutralization step, before the aging step, or after the aging step, and when the α-sulfofatty acid alkyl ester is used. , Α_sulfofatty acid alkyl ester salts.

 The hydrogen peroxide or the compound that generates hydrogen peroxide is not particularly limited, but is preferably an aqueous hydrogen peroxide solution, sodium percarbonate, or potassium percarbonate, and particularly preferably an aqueous hydrogen peroxide solution in terms of cost and effect. From the viewpoint of stability and safety, an aqueous solution of 35 to 50% by mass is preferable. One or more of the above compounds can be used.

 The blending amount of hydrogen peroxide is preferably from 0.1 to 10% by mass, particularly preferably from 0.2 to 9% by mass, more preferably from 0.3 to 8% by mass, based on the blending amount of the monosulfo fatty acid alkyl ester. If the amount based on the amount of the monosulfo fatty acid alkyl ester is less than 0.1% by mass, sufficient bleaching and deodorizing effects may not be obtained. On the other hand, if it exceeds 10% by mass, the amount of water entrained together with hydrogen peroxide increases, so that granulation at a high concentration may be difficult.

In order to improve the solubility of the particles containing the α-sulfofatty acid alkyl ester salt, a solubility improver may be added, and the step of adding the solubility improver is not particularly limited. Examples of the solubility improver include surfactants other than the sulfo fatty acid alkyl ester salt and And water-soluble polymer compounds. As the surfactant, an anionic surfactant, a nonionic surfactant and an amphoteric surfactant are preferred, and a nonionic surfactant and an amine oxide amphoteric surfactant are particularly preferred.

 As the anionic surfactant, a linear alkylbenzene sulfonate is preferred. As the nonionic surfactant, fatty acid methyl ester alkoxylate or fatty acid ethyl alkoxylate obtained by adding alkylene oxide to methyl ester or ethyl ester, or alcohol alkoxylate obtained by adding alkylene oxide to alcohol is preferable. As the water-soluble polymer compound, a compound which functions as a dispersant such as polyacrylic acid or a salt thereof, methylcellulose, propylcellulose, or carboxymethylcellulose is particularly preferable.

 The mass ratio of a solubility improver such as a surfactant or a water-soluble polymer compound to the (sulfo fatty acid alkyl ester salt is preferably 0.01: 1 to 0.8: 1. Less than 0.01. In many cases, the effect is not sufficient, and when it exceeds 0.8, the effect is sufficient, but the amount is large, so that the granulation property may be affected.

 In addition, by including a step of coating the surface modifier with the particles after the aging step, good fluidity and solidification can be obtained. As the surface modifier, zeolite, silicon oxide, clay mineral, metal stone, and inorganic sulfate are preferable. Particularly preferred is zeolite which also contributes as a chelating agent. The solubility can be improved by coating potassium sulfate. Coating can be performed in a fluidized bed apparatus, but may be performed in another apparatus such as a horizontal cylindrical rotating drum. Here, other compounds, such as an aqueous hydrogen peroxide solution and a dye, can also be added.

The content of α-sulfofatty acid alkyl ester salt in the monosulfofatty acid alkyl ester salt-containing particles obtained by the production method of the present invention is preferably from 7 to 80% by mass, particularly preferably from 10 to 75% by mass. %, More preferably 15 to 70% by mass. Production is possible even when the content of the α-sulfofatty acid alkyl ester salt is less than 7% by mass, but the low concentration of the α-sulfofatty acid alkyl ester salt-containing particles of the present invention is low. If the content exceeds 80% by mass, it may be difficult to completely complete the neutralization. Hess also The content of the alkaline powder in the rufofatty acid alkyl ester salt-containing particles is preferably from 10 to 93% by mass, and particularly preferably from 15 to 85% by mass. If the amount is less than 10% by mass, it may be difficult to completely complete the neutralization. There are cases. Further, the content of the surface modifier is preferably 0 to 30% by mass, more preferably 1 to 20% by mass, 2 to 10% by mass, and 3 to 8% by mass, and particularly preferably 4 to 6% by mass. .

 Further, if necessary, a dye or the like can be contained. The content is preferably from 0 to 6% by mass, more preferably from 0.1 to 5% by mass, preferably from 0.2 to 4% by mass, and particularly preferably from 0.3 to 3% by mass. In addition, it is also possible to contain a detergent component and other components to be blended in the detergent described later.

 The concentration of the α-sulfofatty acid alkyl ester salt-containing particles of the present invention can be further increased by incorporating an oil-absorbing carrier. As the oil-absorbing carrier, those having an oil-absorbing capacity of 6 OmL / 100 g or more, particularly 80 mL / 100 g or more, more preferably 10 OmL / 100 g or more, as measured by the method of JIS K 5101 are preferred. Examples of the oil-absorbing carrier include amorphous silicate, silicon oxide, amorphous calcium silicate, amorphous aluminosilicate, magnesium silicate, magnesium carbonate, calcium carbonate, spinel, cordierite, mullite, and starch. Degradation products and the like.

The average particle size of the α-sulfofatty acid alkyl ester salt-containing particles obtained by the production method of the present invention is preferably 100 to 900 m. Particularly preferably, it is 120 to 800 / m. When coarse particles are present, it is preferable to carry out sieving or pulverizing operation to make the particle size uniform. The bulk density is generally 0. 2~1. 4gZcm is ^{3, 0. 3~1. 2 g /} cm 3 are preferred, especially ^{0. 3~1. O g / cm 3} , further from 0.4 to 0 6 g / cm ³ is preferred. The method for measuring the average particle size and the bulk density is the method described in the examples.

 If dusting of the obtained particles becomes a problem, a small amount of nonionic surfactant or the like may be sprayed. As a result, dust generation can be suppressed in order to prevent scattering of fine powder that causes dust generation.

A second invention is a detergent containing particles containing α-sulfofatty acid alkyl ester salt. You. In addition to the monosulfofatty acid alkyl ester salt-containing particles in the detergent, detergent components and other components are included.

 The detergent component includes a detergent component, a bleaching component, a component that improves the productivity and powder properties. The detergent component and other components that can be used in the detergent of the present invention include anionic surfactants, nonionic surfactants, cationic surfactants, amphoteric surfactants, chelating agents (zeolites, organic builder, etc.), Alkaline builder, neutral inorganic builder, anti-redeposition agent, viscosity modifier, softener, reducing agent, bleach, bleach activator, fluorescent brightener, fragrance, enzyme, dye, surface modifier, Examples include a foam inhibitor, an antioxidant, and water.

 The form of the detergent component and other components is not particularly limited, and raw materials such as the above-mentioned detergent components may be used as they are, or may be used as detergent particles. The detergent particles are not particularly limited as long as they include components contributing to cleaning such as the above-mentioned detergent components, and particularly, those containing any of a surfactant, an alkaline builder, and a chelate builder are preferable.

 The mixing weight ratio of the monosulfo fatty acid alkyl ester salt-containing particles to the detergent component and other components in the detergent is preferably from 96: 4 to 4:96, particularly preferably from 95: 5 to 5:95.

 The detergent can be obtained by mixing the monosulfofatty acid alkyl ester salt-containing particles with the detergent component and other components according to a conventional method, and the mixing is preferably performed by dry mixing. In dry mixing, particles containing α-sulfofatty acid alkylester salt, detergent components and other components are charged into a device capable of mixing solids, and the mixing temperature is 5 to 130 ° (: preferably 10 to 1 °). In 2 Ot :, mixing is performed for 0.5 seconds or more, preferably 5 seconds or more, particularly 30 seconds or more The upper limit of the mixing time is not particularly limited The apparatus used for dry mixing is not particularly limited, , A horizontal cylindrical mixer, a V mixer, and a stirring granulator are preferred.

 A third invention is a detergent product in which the particles or detergent containing the monosulfo fatty acid alkyl ester salt is filled in a packaging container made of paper, plastic, or a composite material of paper and plastic.

Containers are made of paper, plastic, and composites of these. plus It is preferable that the tics do not contain chlorine in consideration of the environment. For example

, PE (polyethylene), PP (polypropylene), PET (polyethylene terephthalate) and the like.

 According to the present invention, a high-concentration α-sulfofatty acid alkyl ester salt-containing particle which can easily obtain a high-concentration monosulfofatty acid alkyl ester salt and is excellent in powder properties (fluidity and solidification) during storage Can be obtained.

 EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples. In addition, in the following examples, the percentage of the composition not particularly specified indicates% by mass.

 [Examples 1 to 20, 25, 26, Comparative Examples 1 to 5]

 <Production method>

 (Mixing and neutralization process-fluidized bed equipment)

 Alkaline inorganic powders (potassium carbonate, sodium tripolyphosphate, sodium carbonate, the same applies hereinafter) of the compositions 1 to 8 listed in Table 7 were used as raw materials (excluding coating agents) in fluidized bed equipment (manufactured by Parex Co., Ltd., G 1 att-P〇WREX, Model No. FD-W RT-20) was added with a mass to give a powder layer thickness of 200 mm when allowed to stand. Thereafter, air at the temperature described in Tables 8 to 12 was sent into the fluidized bed, and after confirming that the powder had fluidized, the air was directed toward the powdered bed where the sulfosulfo fatty acid alkyl ester was fluidized. It sprayed from the part. The wind speed in the fluidized bed was adjusted in the range of 0.2 to 2. OmZs while checking the fluidized state.

 The monosulfo fatty acid alkyl ester was sprayed at 60 ° C, and the spray nozzle was a 2-fluid hollow cone nozzle with a spray angle of 70 °. The spray speed was about 400 g / min.

 (Aging process-fluidized bed equipment)

 After the spraying of the monosulfo fatty acid alkyl ester was completed, the temperature of the fluidized bed was changed to the air temperature shown in Tables 8 to 11, and aging was performed for the time shown in Tables 8 to 11.

 (Addition of solubility improver)

When nonionic surfactant ② as a solubility improver was added, the following method was used. The aged granules were charged into a 20-liter Reedige mixer (Matsubo Co., Ltd., Model M-20) through which cold water at 10 ° C was passed through the jacket so that the filling rate was 30% by volume. Thereafter, Nonionic Surfactant ② was added in about 30 seconds while rotating the spindle and the chopper at 150 rpm and 4000 rpm, respectively.

 (Coating process)

 The particles obtained in the above step were placed in a horizontal cylindrical rotating drum having a diameter of 400 mm and a length of 700 mm, and the matured particles and A-type zeolite or potassium sulfate as a coating agent were added thereto to obtain an F r of 0. Mix for 3 minutes at 14.

 (Evaluation of powder properties)

 The powder properties of the coated particles of the monosulfo fatty acid alkyl ester salt were measured by the following methods. The physical properties immediately after coating were the physical properties immediately after coating, and the physical properties over time were measured by placing particles up to 250 mm in an acrylic acrylic container having a diameter of 150 mm and a height of 300 mm, taking out the particles 30 minutes later, and measuring the physical properties of the following evaluation items. The results are shown in Tables 8 to 12.

Evaluation item

 (1) Fluidity: The angle of repose was measured using a turntable type angle of repose analyzer manufactured by Tsutsui Physical and Chemical Instruments. The evaluation was made according to the following evaluation criteria.

 60. Less than… ㊀

 60 ° or more and less than 70 ° ~ △

 Over 70 °…

 (2) Solidification: The mass% of the particles remaining on the top was measured through a 3 # sieve.

 Less than 10%…

 10% or more and less than 40% ~ △

 Do not discharge from 40% or more or acrylic container…

 (3) Measurement of average particle size

Classification was performed using 9-stage sieves and pans with openings of 1680 mm, 1410 urn, 1190 rn, 1 000 m, 710 m, 500 m, 350 fim, 250 m, and 149 m. The classification operation is performed by stacking the sieves with small openings to large sieves on a tray in a pan, and 100 times from the top of the 1680 μη sieve. Put the base sample, cover it, attach it to a one-tap sieve shaker (manufactured by Iida Manufacturing Co., Ltd., tapping: 156 times / min, mouth ring: 290 times), shake for 10 minutes, and then shake each. An operation of collecting the sample remaining on the sieve and the tray for each sieve was performed.

 By repeating this operation, 1410-1680 (1410 m.on), 1190-: L 410 m (1 190 m.on), 1000-1190 m (1000 ^ m.on), 710-1000 / xm ( 710 m.on) 500-7 10 m (500 u.on), 350-500 m (350 m.on), 250-350 (250 / zm.on), 149-250 m (149 ^ m.on) ), Classified samples of each particle size from dish to 149 m (149 m. Ass) were obtained, and the weight frequency (%) was calculated.

 Next, the opening of the first sieve at which the calculated weight frequency is 50% or more is defined as am, the opening of the sieve one step larger than am is defined as bm, and the integration of the weight frequency from the saucer to the sieve of am is calculated. The average particle size (50% by weight) was determined by the following formula, where c% and the weight frequency of a on the sieve were d%.

 (50- (c-d / (logb-loga) X logb)) / (d / (logb-loga)) Average particle size (weight 50%) = 10

 (4) Measurement of bulk density

 The bulk density was measured according to JIS K3362.

 [Examples 21 to 24, 27]

 (Mixing and neutralization process-stirring granulator)

A 20 L Ledige mixer (Matsubo Co., Ltd., manufactured by Matsubara Co., Ltd.) in which the alkaline inorganic powder raw materials (excluding the coating agent) having compositions 1, 2, 7 to 9 shown in Table 7 are passed through a jacket through cold water at 10 ° C. A quantity of 50% by volume (volume: 10L) was charged into Model M-20) (powder temperature: 30 ° C). Thereafter, the spindle and the chopper were rotated at 150 rpm and 6000 rpm, respectively, for 15 seconds and stopped, and then a monosulfo fatty acid alkyl ester (temperature: 60) was added. The operation of stirring the sulfofatty acid alkyl ester into three portions, adding 1Z3 and stirring for 15 seconds was repeated three times, and the whole amount was added (temperature after completion of addition: 90). In addition, α-sulfo fatty acid alkyl ester 1Z The time for adding the three components was about 20 seconds.

 When adding nonionic surfactant ② and linear alkylbenzene sulfonic acid, which are solubility improvers, after addition of α-sulfofatty acid alkyl ester was completed, it was added in about 30 seconds while rotating the main shaft and chopper. .

 (Aging process-stirring granulator)

 The resulting neutralized product was aged in a Loedige mixer. The rotation speed of the main shaft and the chopper was the same as during mixing, and the airflow was introduced from the shaft seal part of the main shaft and the airflow introduction nozzles specially provided on the wall, and aged at the wind temperature and time shown in Table 11.

 (Coating process)

 After aging, the obtained particles are discharged from a stirring granulator, and the aging particles and A-type zeolite (coating agent) are put into a horizontal cylindrical rotating drum of 400 mm in diameter and 700 mm in length. Then mixed with 1 "number 0.14 for 3 minutes.

 (Evaluation of powder properties)

 After aging, the α-sulfofatty acid alkyl ester salt-containing particles subjected to the coating step were evaluated for physical properties in the same manner as described above. The results are shown in Table 11 together.

 [Examples 28 to 38]

 (Bleaching and coloring process)

 The particles obtained in the above Examples were sprayed with an aqueous solution of hydrogen peroxide, a dye and a fragrance (all at a temperature of 20) in the amounts shown in Table 13 in a horizontal cylindrical rotary drum. Rotation conditions were Fr number 0.14, and spraying was performed using a Kuramata sprayer.

 Thereafter, the surface modifier in the amount shown in Table 13 was used as a surface modifier in a horizontal cylindrical drum, and was coated with bleached and colored α-sulfofatty acid alkyl ester salt-containing particles. The obtained mono-sulfo fatty acid alkyl ester salt-containing particles were evaluated in the same manner as described above. Table 13 shows the evaluation results.

 [Examples 39 to 58]

 (Mixing with other particles)

The particles obtained in the above Examples were mixed in the mixed particles and ratios shown in Tables 14 to 18. For mixing, the particles were put into a horizontal cylindrical drum (diameter 400 mm, length 700 mm,? 1 "number 0.14), mixed for 2 min, and then discharged to obtain a mixed product. mixture The product was evaluated in the same manner as described above. The evaluation results are shown in Tables 14-18. The mixed particles 1 to 5 are shown below.

 Composition of mixed particles and manufacturing method>

 Mixed particles 1: NABION 15 (trade name, manufactured by Kuchiichi Dia Co., Ltd.) was used. The composition is shown in Table 1 (see Rabdia catalog Nab / HC 07.2000).

 [table 1]

 Mixed particle 1 composition (% by mass) Refer to Kuchiichidia catalog

 (Mixed particles 2)

From the compositions shown in Table 2, raw materials excluding type III zeolite and fragrance were blended at a predetermined ratio to prepare a slurry having a water content of 40% and a temperature of 70 ° C. LAS-Na was charged with LAS-H and NaOH to produce LAS-Na in the slurry. The slurry was transferred to the top of the drying tower (diameter 2 m, effective length 5 m) by a plunger pump, and then sprayed into the tower from the pressurized nozzle at a pressure of 30 kgZcm ² and dried. The temperature inside the drying tower was 260 ° C at the hot air inlet, and the exhaust air temperature during operation was 100 ° C. The powder obtained from the bottom of the tower and the A-type zeolite were mixed, and a fragrance was sprayed to obtain mixed particles 2. The temperature of the obtained mixed particles 2 was 40 ° (:, the bulk density was 0.40 g / cm ^3. The composition of the mixed particles 2 is shown in Table 2.

[Table 2]

 Mixed particle 2 composition (The numbers in the table are% by mass)

 (Mixed particles 3)

 Of the compositions (dry powder compositions) shown in Table 3, the raw materials excluding the A-type zeolite of the coating were blended at a predetermined ratio to prepare a slurry having a water content of 40% and a temperature of 70 ° C. LAS-K was fed with LAS-H and KOH to produce LAS-K in the slurry.

The slurry was transferred to the top of the drying tower (diameter 2 m, effective length 5 m) by a plunger pump, and then sprayed into the tower from the pressurized nozzle at a pressure of 30 kgZcm ² and dried. The temperature inside the drying tower was 260 ° at the inlet of hot air (: The exhaust air temperature during operation was 100 ° C. The powder obtained from the bottom was coated with A-type zeolite as a coating agent. As a result, a dry powder having the composition shown in Table 3 was obtained.

The obtained dry powder, water, and nonionic surfactant were mixed at a ratio of 88.44: 0.89: 3.33 (mass ratio) in a kneader (a kneading machine, manufactured by Kurimoto Tetsusho Co., Ltd., KRC Knee). Into a kneader, Model S-4) to obtain a kneaded mixture at a temperature of 60. The capacity was 150 kgZhr (time, hereinafter the same) as a kneaded mixture. The kneaded mixture was poured into a pellet (Yuichi Baudal, die hole diameter l Ommc)) to form a pellet-like solid having a diameter of about 10 mm and an average length of 10 to 3 Omm. A Fitz mill (manufactured by Hoso Power Micron Co., Ltd.) in which the obtained pellet-shaped solid detergent and A-type zeolite were arranged in three stages in series with cold air at 15 at a ratio of 92.66: 4.00 (mass ratio), DKA—Type 3, 1st stage: screen diameter 12mmc |, 2nd stage: screen diameter 6mm (i), 3rd stage: screen diameter 2.3mm ^, rotation speed all stages 47 OO r pm) Milled at 190 kg / hr. The obtained pulverized particles had an average particle size of 550 / im, a repose angle of 50 °, and a bulk density of 0.75 g / cm ³ . The obtained milled particles are placed on a horizontal cylindrical rolling drum (0.70 m in diameter, 1.40 m in length, 3 ° incline, 5 lmmx in height, 5 OmmX, with 15 baffles with a length of 35 Omm) and A type zeolite. Nonionic surfactant and fragrance were sprayed inside the container continuously, and mixed particles 3 were obtained. The mass ratio of the pulverized product charged into the horizontal cylindrical rolling drum, A-type zeolite: sprayed nonionic surfactant: perfume was 96.66: 2.90: 0.34: 0.10. The obtained mixed particles had an average particle size of 550 m, an angle of repose of 40 °, and a bulk specific gravity of 0.82 gZcm ³ . Table 4 shows the composition of the mixed particles 3 finally obtained.

3] Mixed particles 3 Dry powder composition (The numbers in the table are mass%)

(Mixed particles 4)

 In Table 5 below, a main type of A-type zeolite, white bonbon, sodium carbonate ① equipped with a plow-blade shovel, and a clearance of 5 mm between the shovel and the wall. Reedige mixer (Matsupo Co., Ltd., M (20 type) was added in such an amount that the volume became 50% by volume (powder temperature: about 30 ° C). Thereafter, the main shaft and the chopper were rotated at 200 rpm and 600 rpm, respectively, for 30 seconds to mix the powder.

 Melt and mix the nonionic surfactant ス テ and 12-hydroxystearic acid at 85 ° C in advance, and after mixing the powder, turn the non-ionic surfactant ① and 12-hydroxy The molten mixture of stearic acid was added in about 60 seconds.

 After completion of the addition of the molten mixture, the main shaft and the rotation of the chopper were continued while the divided A-type zeolite was added, and the mixture was stirred for 90 seconds. Thereafter, the coating type A zeolite was added, stirred for 30 seconds, and taken out of the Loedige mixer.

 The obtained particles were passed through a sieve having an opening of 2000 tm to obtain mixed particles 4.

 Five ]

4 mixed particles composition (the numbers in the table are mass%)

 (Mixed particles 5)

From the compositions shown in Table 6 below, the raw materials excluding the coating type A zeolite were blended at a predetermined ratio to prepare a slurry having a water content of 50% and a temperature of 80 ° C. The slurry was spray-dried in a drying tower under the same conditions as for the mixed particles 2, and the dried powder obtained from the bottom of the slurry and the coating type A zeolite were mixed to obtain mixed particles 5. The temperature of the obtained mixed particles 5 was 4 O :, and the bulk density was 0.4 g / cm ³ . 6]

5 composition of mixed particles (the numbers in the table are% by mass)

 Filling the packaging container with particles>

 The particles obtained in Examples 1 to 58 were filled in the following packaging container.

Packaging container: The packaging container size was 20 Omm width x 10 Omm depth x 15 Omm height, and the material used was a laminated paper made of polyethylene on paper.

 Although stored for 4 weeks at 20 ° C and 60% relative humidity, none of them solidified and had good powder properties.

The compounding amount shown in the following table is shown by mass%. The molar ratio between the α-sulfofatty acid alkyl ester and the alkaline inorganic powder is represented by the molar ratio of the pure component. The alkaline inorganic powders shown here are lithium carbonate, sodium carbonate, and sodium tripolyphosphate.

[Table 7]

 Composition Composition Composition Composition Composition Composition Composition Raw material

 1 2 3 4 5 6 7 8 9 α-sulfo fatty acid

 39.28 50.51 50.51 61.73 72.96 50.51 39.28 50.51 39.28 Alkyl ester

 Potassium carbonate 6.06 5.05 10.10 10.10 10.10 5.05 6.06 5.05 6.06 Trifo. Sodium riphosphate 5.88 5.88 ― 2.35 2.35 5.88 I―Iso sodium carbonate①

 43.78 33.56 34.39 20.82 9.59 33.56 45.16 33.94 45.16 (pulverized light ash)

 ® Nonionic surfactant

 I-----4.5 4.5 ― ②

%

 Straight chain alkyl

 ------One 4.5 4.5

 ΑType 'Olite Shilton Β

 5.00 5.00 5.00 5.00 5.00-5.00 3.00 3.00 (Coating agent)

 Potassium sulfate

 ― ― ― ― ― 5.00 ― 3.00 2.00 (Coating agent)

 100 100 100 100 100 100 100 100 100 α-sulfo fatty acids

 Alkyl ester:

 1: 4,6 1: 2.8 1: 3.0 1: 1.7 1: 0.9 1: 3.0 1: 4.9 1: 2.9 1: 4.9 Alkaline inorganic powder

(Molar ratio)

8]

 Example 1 Example 2 Example 3 Example 4 Example 5 Aging equipment Fluidized bed Fluidized bed Fluidized bed Fluidized bed Fluidized bed Composition 1 Composition 1 Composition 1 Composition 2 Composition 2 Fluidized bed wind temperature during mixing (° c) 20 20 30 20 20 Wind temperature (° C) 20 30 30 20 30 Aging condition

 Time (sec) 240 240 180 420 420 Average particle size (μηι) 350 350 350 450 450 Powder properties

Bulk density (g / cm ³ ) 0.5 0.5 0.5 0.5 0.5 0.5 Repose immediately after 〇 〇 〇 〇 直 後 Solidification immediately after 直 後 〇 〇 〇 〇 Powder properties

 Angle of repose over time 〇 〇 〇 〇 固 Solidification over time 〇 〇 〇 〇 9 9 9]

 Example 6 Example 7 Example 8 Example 9 Example 10 Aging equipment Fluidized bed Fluidized bed Fluidized bed Fluidized bed Fluidized bed Composition 2 Composition 2 Composition 2 Composition 2 Composition 3 Fluidized bed air temperature during mixing (° C) 20 30 30 40 20 Wind temperature (° C) 40 30 40 40 20 Aging condition

 Time (sec) 360 360 300 300 360 Average particle size (μ πι) 470 450 450 470 400 Powder properties

Bulk density (g / cm ³ ) 0.5 0.5 0.5 0.5 0.5 0.5 Repose immediately after 〇 〇 〇 〇 o Solidification immediately after 〇 〇 〇 〇 〇 Powder properties

Angle of repose over time 〇 〇 〇 〇 o Solidification over time 〇 〇 〇 〇 〇

[Table 10]

[Table 11]

 Example

 16 17 18 19 20 21 22 23 24 25 26 27 Stirring Stirring Stirring Stirring Flowing Flowing Flowing Flowing Flowing Flowing Aging equipment Granulation Granulation Granulation Granulation Granulation layer Layer

 Apparatus apparatus apparatus apparatus apparatus composition composition composition composition composition composition composition composition composition composition composition composition composition

 4 4 5 5 6 2 1 7 8 7 8 9 Fluidized bed during mixing

 20 20 20 20 20 One-one-20 20-Wind temperature (° c)

 Wind temperature

Mature 20 30 20 30 40 20 10 10 10 30 30 10 Composition (° C)

Article

Case Time (sec) 600 480 720 600 360 60 240 180 180 360 360 240 Average particle size

(Powder 500 500 550 550 470 350 320 500 550 600 620 500 body, μm)

Bulk density

0.5 0.5 0.5 0.5 0.4 0.7 4 0.7 0.7 0.7 0.5 0.5 0.7 (g / cm ³ )

 Immediately after

 〇 o 〇 〇 〇 〇 〇 〇 〇 〇 〇 角 Angle of repose

 Immediately after

Powder 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 Solidification

Object

Sex 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 角 〇 Angle of repose

 Aging

〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 Solidification [Table 1 2]

13 ]

 Example

 Mass% 28 29 30 31 32 33 34 35 36 37 38 Aged particles 1 4 10 16 18 4 10 22 23 25 27

(Example) 90.5 89.0 89.0 88.0 88.0 92.6 92.6 90.9 90.9 90.9 90.9 Hydrogen peroxide

 4.5 6.0 6.0 7.0 7.0 0.3 0.3 4,0 4.0 4.0 4.0 Aqueous solution

 Pigment-----2.0 2.0----Fragrance-----0.1 0.1 0.1 0.1 0.1 0.1

A type seolite

 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 Shilton B

 α μ 1 100 100 100 100 100 100 100 100 100 100 100 Average particle size

 380 500 430 550 590 460 410 350 540 630 550

(Γθ)

 Peace

 0.5 0.5 0.5 0.5 0.4 0.5 0.5 0.7 0.7 0.5 0.7

(g / cm ^a )

 Immediately after

 〇 〇 〇 〇 〇 O 〇 〇 〇 〇 〇 Angle of repose

 Immediately after

 Powder 〇 〇 〇 〇 O 〇 〇 〇 〇 〇 O solidification

 Object

 Sex 〇 〇 o 〇 O 〇 o 〇 〇 〇 〇 Angle of repose

 Aging

〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 化 Solidification [Table 14]

[Table 15]

16]

 Example 47 Example 48 Example 49 Example 50 Example 28:20 Example 34:33 Example 28:33 Example 34: 15

 Particle mixing ratio Mixed particles 1:60 Mixed particles 1:20 Mixed particles 1:47 Mixed particles 1:65

 (%) Mixed particle 4:10 Mixed particle 4:20 Mixed particle 4:20 Mixed particle 4:20

 Mixed particle 5: 10 Mixed particle 5:27 Immediately after angle of repose 〇 O O 〇 Powder

 Solidification immediately after body O 〇 〇 〇 物 物 O 〇 性

Solidification over time 〇 〇 〇 〇 [17]

 The raw materials used in the examples are shown below.

 (1) α-sulfo fatty acid alkyl ester

The fatty acid methyl ester used as the raw material was purified by reducing the iodine value by hydrogenating a fatty acid methyl ester (trade name: Edeno MEPA MY (manufactured by Cognis)) obtained by esterifying palm oil. Was used. The hydrogenation treatment is carried out in the usual manner by adding 0.15% of SO-850 (trade name, manufactured by Sakai Chemical Co., Ltd.) as a hydrogenation catalyst to the fatty acid methyl ester at 170 ° C for 8 hours. Was. After the hydrogenation treatment, the catalyst was removed by filtration. The method for producing the hypersulfofatty acid alkyl ester was based on the method disclosed in Example 1 of JP-A-2001-64248, and extracted after the esterification step to obtain a hypersulfofatty acid alkyl ester. Table 19 shows the carbon distribution and properties of the raw material fatty acid methyl ester. 19]

The resulting monosulfofatty acid alkyl ester had a purity of 89.1%. The color tone of the sodium sulfo fatty acid alkyl ester was 900 when measured with a Kret photoelectric meter using a No. 42 blue-filled No. 42 optical path length of a 5% ethanol solution or a 5% aqueous solution using a 4 Omm optical path length. . The calculation was performed on the assumption that the average molecular weight was 366. (2) Sodium carbonate ①: Asahi Glass Co., Ltd., light ash, pure content 99%, bulk density 0.55 gZcm ³ crushed light ash to an average particle size of 10-60 m

Sodium carbonate: manufactured by Asahi Glass Co., Ltd., grain ash, pure content 99%, bulk density 1.07 g / cm ³

(3) Potassium carbonate: Asahi Glass Co., Ltd., food grade, crushed, 99% pure, bulk density 77 g / cm ³

(4) Sodium tripolyphosphate: Taihei Chemical Co., Ltd., food grade, 85% pure, bulk density 0.97 g / cm ³

(5) Zeolite A: manufactured by Mizusawa Science Co., Ltd., trade name Shilton B, bulk density 0.30 gZcm ³

(6) Hydrogen peroxide: Junsei Chemical Co., Ltd., first-class reagent, aqueous solution containing 35% hydrogen peroxide (7) Nonionic surfactant I: Alcohol ethoxylate obtained by adding an average of 15 moles of ethylene oxide to an alcohol having 12 to 14 carbon atoms (purity = 90%, the remainder is unreacted alcohol, PEG (polyethylene glycol), water, etc.)

 (8) Nonionic surfactant I: Fatty acid methyl ester ethoxylate obtained by adding an average of 15 mol of ethylene oxide to methyl ester (trade name: CE-1618, manufactured by FPG) (unreacted methyl ester, reactive solid (Including catalyst, PEG, etc.)

(9) Acrylic acid / maleic acid copolymer Na: manufactured by Nippon Shokubai Co., Ltd., trade name: Aquaric TL-1400 (40% pure solution in water)

 (10) LAS-H: Raibon LH-200 (manufactured by Lion Corporation), linear alkylbenzene sulfonic acid having an alkyl group having 10 to 14 carbon atoms (AI = 96%

The rest is unreacted alkylbenzene, sodium sulfate, water, etc.), used as LAS-Na, LAS-K.

 (11) Stone: C16: C18: TMD (ester mixture of C10-20) = 1: 3: 1 sodium fatty acid (AI = 67%)

 [Production method]

 Fatty acid methyl ester at 40-60 ° C (Pastel M-C * 〇, manufactured by Liono Leo Chemical Co., Ltd.) 1576 kg / hr, 48% NaOH aqueous solution at 40-60 ° C 445 kg / hr, water (Lion Chiba 336 kg Z hr is continuously introduced into the mixing pump, and the oxidation reaction proceeds for 9 to 10 minutes while maintaining the temperature at 110 to 130 ° C with a shell and tube type heat exchanger and preheater. (Reaction rate 99.5 to 99 • 8%). Next, the reaction mixture was introduced into a flash evaporator having an overhead pressure of 0.2 to 0.6 kPa and an overhead temperature of 98 to: L00, and methanol as a reaction product was evaporated at a residence time of 40 minutes. Finally, the stone from which the methanol was removed was introduced into a stirring tank having paddle-type stirring blades, and while maintaining the temperature at 98 ° C with stirring for a residence time of 140 minutes, 80t: hot water was added, and the stone concentration was 66%. The concentration was adjusted to be ~ 67%.

 The stone thus obtained has an AI of 66-67%, and as impurities, about 0.01% fatty acid, about 0.2% unreacted fatty acid ester, about 0.2% Na〇H, It contained 0.4% methanol.

(12) AOS— K: α-olef with 14: 16: 18 = 15: 50: 35 carbon atoms A mixture of potassium sulfonate and potassium hydroxyalkylsulfonate (purity 70%, potassium sulphate sulphonate: potassium hydroxyalkylsulphonate ratio 7: 3, the remainder unreacted α-sulphate refine, sodium sulphate, Salt, sodium hydroxide, water, etc.)

 [Production method]

25 ° C freerefin (Dialen 148, manufactured by Mitsubishi Chemical Corporation) is continuously introduced into the TO reactor (TO-500, manufactured by Lion Corporation, film-type reactor) with a capacity of 970 kgZhr. Then, a sulfonation reaction was carried out by contacting the inside with S で₃ gas to obtain a sulfonated product containing about 35 t: of α-refin sulfonic acid and impurities (mainly sultone). A neutralization reaction was performed by adding 630 kg / hr of caustic force (52% aqueous solution) to 1370 kg / hr of the sulfonated product to obtain potassium olefin sulfonate containing impurities. In order to hydrolyze the sultone in these impurities, the temperature is raised to 140 ° C through a shell-and-tube heat exchanger, and further maintained at 170 ° C through 1.4MPa steam in a reaction tube to promote hydrolysis. I let it. Thereafter, flash concentration and dehydration were performed at a pressure of IMP a to reduce the water content to about 27%.

 The pure fraction of AOS-K obtained in this way is usually 66-74%, the main components of which are potassium hexafluorosulfonate (about 70%) and hydroxyalkylsulfonic acid potassium (about 30%). (LK value of 10% solution) 70, free alkali content (KOH) 1.8% (vs. AOS-K pure content).

 (13) Calcium carbonate: Junsei Chemical Co., Ltd., reagent grade calcium carbonate

 (14) Sodium silicate: Nippon Kagaku Kogyo, JIS No. 1 sodium silicate

 (15) Pigment: DAINICHI SEIKA KOGYO, ultramarine

 (16) Potassium sulfate: Ueno Pharmaceutical Co., Ltd., obtained by grinding potassium sulfate to 20-30

 (17) White Carbon: Tokuyama N, manufactured by Tokuyama Soda Co., Ltd.

 (18) 12-hydroxystearic acid: KY Trading Co., Ltd., 85% pure

(19) Fragrance: as shown in JP-A-2002-146399, [Table 11] to [Table 18] Scent composition A

Claims

The scope of the claims

 1. The step of mixing and neutralizing the alkyl sulfo fatty acid ester and the alkaline powder, and the step of ripening while mixing and neutralizing the obtained mixed and neutralized powder in an apparatus equipped with an airflow generator. A process for producing monosulfofatty acid alkyl ester salt-containing particles, comprising:

 2. The method according to claim 1, further comprising the step of bleaching the sulfofatty acid alkyl ester and the thiosulfofatty acid alkyl ester salt with hydrogen peroxide or a compound generating hydrogen peroxide. The production method according to item 1.

 3. The method according to claim 1 or 2, wherein the step of mixing and neutralizing the α-sulfofatty acid alkyl ester and the alkaline powder is performed in a fluidized bed.

4. A sulfo fatty acid alkyl ester obtained by contacting a fatty acid alkyl ester with a sulfonating gas in the presence of a coloring inhibitor to sulfonate the sulfonated fatty acid alkyl ester and esterifying the obtained sulfonated product with a lower alcohol. The manufacturing method according to any one of claims 1 to 3, wherein the manufacturing method is a tellurium.

5. α-Sulfo fatty acid alkyl ester salt-containing particles produced by the production method according to any one of claims 1 to 4, containing 7 to 80% by mass of an α-sulfo fatty acid alkyl ester salt.

 6. A detergent comprising the α-sulfofatty acid alkyl ester salt-containing particles according to claim 5.

 7. A detergent product wherein the particles containing a-sulfofatty acid alkyl ester salt according to claim 5 or the detergent according to claim 6 are packed in a packaging container made of paper, plastic, or a composite material of paper and plastic.