JP2006274156A - Manufacturing method of high purity anion surfactant powder (bead) - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a manufacturing method of a high purity anion surfactant powder (bead) with a high yield requiring no large scale drying facility and a large quantity of thermal energy, without accepting a lot of thermal history, and requiring no specific solvent and additive. <P>SOLUTION: In this manufacturing method of a high purity anion surfactant powder (bead), a crude anion surfactant powder (bead) is treated by contacting with an extraction solvent, then the anion surfactant powder (bead) is separated from the extraction solvent, and dried. This product contains the anion surfactant not less than 90 wt.%. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a high-purity anionic surfactant granular material. More specifically, for example, a high-purity anion that can be suitably used for clothes detergents, kitchen detergents, toothpaste foaming agents, shampoo powders, polymer polymerization emulsifiers, pharmaceutical emulsifiers, cosmetic emulsifiers, cement foaming agents, and the like. The present invention relates to a method for producing a surfactant granular material.

  Anionic surfactants, when mixed with other surfactants or builders, are used in laundry detergents, kitchen detergents, toothpaste foaming agents, pharmaceutical emulsifiers, cosmetic emulsifiers, and other detergents. ing.

Conventionally, in order to obtain a relatively high-purity anionic surfactant powder or granular material, an anionic surfactant aqueous solution, water slurry or paste (in addition, an anionic surfactant aqueous solution, water slurry or paste, etc. are handled in the same manner). After that, after removing impurities (Patent Document 1, Patent Document 2, and Patent Document 3) in the state of anionic surfactant aqueous solution as an example), it is dried and / or granulated by various methods. High purity anionic surfactant powder and a method of removing impurities simultaneously with and / or after drying (Patent Document 4, Patent Document 5, Patent Document 6, Patent Document 7) A method for obtaining an anionic surfactant is known.
JP-A-53-68728 U.S. Pat. No. 4,322,367 JP-A-48-52687 JP-T 6-504526 US Pat. No. 6,455,488 Japanese Patent Laid-Open No. 5-331496 JP 2002-129194 A

  In the method of obtaining the anionic surfactant powder particles by removing impurities in the state of the anionic surfactant aqueous solution and then drying, if the anionic surfactant aqueous solution has high moisture, large-scale drying is performed in the drying process. Requires equipment and significant heat energy. For this reason, it is preferable to treat with an aqueous solution having a low water content as much as possible. However, when the water content becomes low, not only does the viscosity increase rapidly, but an emulsion or gel is often formed, which makes it difficult to separate the extraction solvent and impurities. In order to avoid this, there are problems that it is necessary to limit the extraction solvent, to use a mixture of two or more extraction solvents, or to use additives other than the extraction solvent for the purpose of viscosity reduction / fluidization. It was.

  On the other hand, in the method of removing impurities simultaneously with and / or after drying, a large amount of carrier gas is required, and the processed material receives a lot of heat history to remove impurities in addition to a simple drying operation. become. In addition, the anionic surfactant is subjected to a thermal history, thereby increasing the concern that impurities are generated by hydrolysis in the presence of side reactions and water / water vapor, and the stability of quality during long-term storage is reduced. There was a problem that an unpleasant smell and taste were developed.

  An object of the present invention is to obtain a high-purity anionic surfactant granular material in a high yield without requiring a large-scale drying facility and a large amount of heat energy, and without receiving a lot of heat history. It is to provide a manufacturing method that can be used.

  The present inventors have found that impurities can be removed very effectively in a short time by solid-liquid extraction of the anionic surfactant granules and the extraction solvent, and high-purity anionic surfactant granules can be obtained. I found it.

  That is, the present invention provides an anionic surfactant obtained by subjecting a crude anionic surfactant granular material to contact treatment with an extraction solvent, separating the anionic surfactant granular material from the extraction solvent, and further drying. Is provided. The manufacturing method of the highly purified anionic surfactant granular material containing 90 weight% or more is provided.

  In the method of the present invention, the impurities in the anionic surfactant can be efficiently extracted at a low temperature by solid-liquid extraction of the crude anionic surfactant powder particles with an extraction solvent. And the extraction solvent can be easily separated into solid and liquid by a technique such as filtration. By drying the extraction solvent remaining in the anionic surfactant powder, the conventional high-purity anionic surfactant powder can be obtained in a very short time. A high-quality / high-purity anionic surfactant powder granule with less heat history than the granule can be obtained.

  According to the present invention, a small-scale drying facility with less heat energy can be obtained by contacting a crude anionic surfactant powder with an extraction solvent without going through a low-concentration anionic surfactant aqueous solution. High-purity anionic surfactant powder with little thermal history, no side reactions or water / water vapor hydrolysis, excellent long-term storage stability, and almost no odor or taste The body can be obtained in a very short time. Moreover, according to this invention, it is not necessary to limit an extraction solvent or to add additives, such as a viscosity reducing agent, and can use a general purpose extraction solvent. Furthermore, since it is a solid-liquid extraction operation using an anionic surfactant powder (solid) and an extraction solvent (liquid), it is very easy to separate the anionic surfactant from the extraction solvent compared to liquid-liquid extraction. There is an advantage of being.

[Anionic surfactant]
The anionic surfactant used in the present invention is not particularly limited, but alkyl or alkenyl sulfate, polyoxyalkylene alkyl or alkenyl ether sulfate, alkylbenzene sulfonate, α-olefin sulfonate, α-sulfo fatty acid salt Or ester, alkyl, or alkenyl ether carboxylate etc. are mentioned. Among these, one or more selected from the group consisting of alkyl or alkenyl sulfates represented by the following formula (I) and polyoxyalkylene alkyl or alkenyl ether sulfates represented by the following formula (II) Is preferred.

(R ¹ O—SO ₃ ) _p M ¹ (I)
(Wherein R ¹ is a linear or branched alkyl or alkenyl group having 8 to 24 carbon atoms, M ¹ is a cation, and p is the valence of M ¹ and represents 1 or 2)
(R ² O— (AO) _m SO ₃ ) _q M ² (II)
(Wherein R ² represents a linear or branched alkyl group or alkenyl group having 8 to 24 carbon atoms, A represents an alkylene group having 2 to 4 carbon atoms, and m A's may be the same or different. even better .m is the number of from 0.05 to 20 showing an average addition mole number of alkylene oxide .M ² cation, q is 1 or 2 a valence of M ^2.)
In general formulas (I) and (II), R ¹ and R ² preferably have 8 or more carbon atoms from the viewpoint of the caking resistance of the powder, and 20 or less carbon atoms from the viewpoint of the solubility of the powder or the like. preferable. Therefore, the carbon number is preferably 8-20, and more preferably 10-18. A is preferably an alkylene group having 2 to 4 carbon atoms, particularly 2 carbon atoms. m is preferably from 0.05 to 2, more preferably from 0.1 to 1, and particularly preferably from 0.2 to 0.8 from the viewpoint of obtaining excellent powder characteristics and improving the caking resistance of the granular material. preferable. M ¹ and M ² are preferably an alkali metal atom such as Na or K, an alkaline earth metal atom such as Ca or Mg, or an alkanol-substituted or inorganic-substituted ammonium group, and more preferably an alkali metal atom, particularly Na.

  The alkyl or alkenyl sulfate represented by the above formula (I) is obtained, for example, by sulfating and neutralizing an alcohol having 8 to 24 carbon atoms, preferably 8 to 20 carbon atoms (hereinafter referred to as higher alcohol). Also. The polyoxyalkylene alkyl or alkenyl ether sulfate represented by the formula (II) is, for example, an alkylene oxide such as ethylene oxide and propylene oxide added to a higher alcohol with an average addition mole number of 0.05 to 20, preferably 0.05 to It is obtained by sulfating and further neutralizing an alkylene oxide adduct of a higher alcohol added so as to be 2.

  Sulfation and neutralization can be performed by known methods. The sulfating agent used for sulfation is preferably sulfur trioxide or chlorosulfonic acid. When using sulfur trioxide gas, it is usually diluted with an inert gas, preferably dry air or nitrogen, and a sulfur trioxide gas concentration of 1 to 8% by volume, preferably 1.5 to 5% by volume of gas. Used as a mixture. Examples of the neutralizing agent include sodium hydroxide, potassium hydroxide, sodium carbonate and the like.

[Rough anionic surfactant powder]
The crude anionic surfactant powder may contain various components shown in the following (1) to (3) in addition to the anionic surfactant.

(1) Water-soluble inorganic salt Examples of the water-soluble inorganic salt include sodium chloride, sodium sulfate, sodium carbonate and the like. The content of the water-soluble inorganic salt in the anionic surfactant powder is not particularly limited, but from the viewpoint of keeping the solid content of the anionic surfactant high, it is 8 parts by weight or less with respect to 100 parts by weight of the anionic surfactant. , Preferably 5 parts by weight or less, more preferably 2 parts by weight or less.

(2) Surfactants other than anionic surfactants Surfactants other than anionic surfactants can be contained. Examples of the surfactant other than the anionic surfactant include a cationic surfactant and a nonionic surfactant.

(3) Other additives Examples of other additives include alkaline agents such as silicates and carbonates, divalent metal ion scavengers such as citrates and zeolites, and prevention of recontamination such as polyvinylpyrrolidone and carboxymethylcellulose. Agents, anti-caking agents, antioxidants, and the like. Such other additives can be used as long as the object of the present invention is not impaired.

  The shape of the crude anionic surfactant powder is not particularly limited, but powder, needle, flake, noodle, granule, pellet, tablet and the like can be used. Among these, granules and pellets are preferable from the viewpoints of ease of handling, ease of solid-liquid separation, and ease of extraction.

  The average particle diameter of the crude anionic surfactant powder is preferably 0.1 mm or more, more preferably 0.2 mm or more, and more preferably 0.5 mm or more from the viewpoint of ease of handling and solid-liquid separation. Particularly preferred. Moreover, 3 mm or less is preferable from a viewpoint of the ease of extraction, 2 mm or less is further more preferable, and 1.5 mm or less is especially preferable. In addition, the average particle diameter in this invention is measured from the weight fraction by the size of the mesh after vibrating for 5 minutes using the standard sieve of JISZ8801.

The bulk density of the crude anionic surfactant powder, from the viewpoint of reducing the scale of equipment, preferably 400 kg / m ³ or more, more preferably 500 kg / m ³ or more, 600 kg / m ³ or more is particularly preferable. From the viewpoint of ease of production, it is preferably 1000 kg / m ³ or less, more preferably 900 kg / m ³ or less. The bulk density in the present invention is a value determined by a method defined in JIS K 3362.

  The water content of the crude anionic surfactant powder is preferably 3% by weight or less, more preferably 2.5% by weight or less, and particularly preferably 2.0% by weight or less from the viewpoint of extraction efficiency. Further, from the viewpoint of reducing the amount of dust (fine powder generated during transportation / handling), it is preferably 0.3% by weight or more, more preferably 0.5% by weight or more, and particularly preferably 1.0% by weight or more. preferable. The water content of the granular material is measured by a method such as a heat loss method, a distillation method, or a Karl Fischer method (JIS K 0068). The water content in this specification was measured by the Karl Fischer method (JIS K 0068). Value.

  From the viewpoint of effectively exhibiting the function of the anionic surfactant itself, the crude anionic surfactant granular material is 80% by weight or more, preferably 90% by weight or more, more preferably 90% by weight or more based on the total amount of the granular material. Contains 95% by weight or more.

  From the viewpoint of handling, the fluidity of the crude anionic surfactant powder is preferably 10 seconds or less, and more preferably 8 seconds or less. The measuring method of the fluidity of the anionic surfactant powder particles in the present invention is the time required for 100 mL of the powder particles to flow out of the bulk density measurement hopper defined in JIS K 3362.

  From the viewpoint of improving the quality and value of the product and the blended product, APHA is preferably 50 or less, more preferably 30 or less, and particularly preferably 15 or less. Further, from the viewpoint of ease of production, APHA is preferably 3 or more, more preferably 5 or more, and particularly preferably 10 or more. The hue is measured by a method of JIS K0071 using a 10% by weight aqueous solution of an anionic surfactant granular material.

  The method for producing the crude anionic surfactant powder used in the present invention is not particularly limited, but a method of simultaneously performing drying and granulation is preferable. Specifically, in a granulator having a stirring blade and a crushing blade. There is a method of granulating simultaneously with drying while adding an anionic surfactant aqueous solution to the powder raw material under reduced pressure. Moreover, when adding the anionic surfactant aqueous solution, a powder raw material may be added in advance to the granulator.

  The water content of the aqueous anionic surfactant solution used here is preferably 20 to 40% by weight from the viewpoint of fluidity and reducing the energy load during drying.

  The anionic surfactant aqueous solution may contain a water-soluble inorganic salt. Examples of the water-soluble inorganic salt include sodium chloride, sodium sulfate, sodium carbonate and the like. These water-soluble inorganic salts may be added as they are, but may be by-produced by reaction. For example, when NaClO (sodium hypochlorite) is added to an anionic surfactant aqueous solution for the purpose of improving the hue, NaCl (sodium chloride) is by-produced. Thus, sodium hypochlorite can be added and sodium chloride can also be by-produced as an inorganic salt.

  The unreacted substance contained in the anionic surfactant aqueous solution is not preferable because it causes a decrease in purity and the caking property of the granular material. However, it is acceptable if it is 5% by weight or less, more preferably 2. % By weight or less. Here, the unreacted material includes not only higher alcohols that have not been sulfated, but also alkoxylates, as well as trace amounts of hydrocarbons and wax by-produced from the reaction.

  The powder raw material used in this production method is preferably one containing at least one selected from the group consisting of a surfactant, a water-soluble inorganic salt and a water-insoluble inorganic salt. It is more preferable to use a part or a pulverized part of the powder as a powder raw material. Examples of the surfactant, water-soluble inorganic salt, and water-insoluble inorganic salt in the powder raw material include those exemplified as those contained in the above-mentioned anionic surfactant. The particle size of the powder raw material is preferably 0.3 mm or less, more preferably 0.2 mm or less, and particularly preferably 0.1 mm or less, from the viewpoints of drying speed and ease of particle size control of the final granulated product and handling properties.

  Examples of the pulverizer used when obtaining the powder raw material include, for example, an atomizer (manufactured by Fuji Paudal Co., Ltd.), Fitzmill (manufactured by Dalton Co., Ltd.), Pulverizer (manufactured by Dalton Co., Ltd.), power mill (Powrec ( Co., Ltd.) and Comil (Quadro).

  In the above production method, the temperature of the granule when granulating simultaneously with drying may require a high vacuum if the temperature is too low, and may require a large amount of energy. The heat source is necessary, and the risk of thermal decomposition increases, so 35 ° C. or higher is preferable, 40 ° C. or higher is more preferable, and 45 ° C. or higher is particularly preferable. Moreover, 85 degrees C or less is preferable, 75 degrees C or less is still more preferable, and 70 degrees C or less is especially preferable. In addition, it is preferable to perform granulation simultaneously with drying while controlling the temperature change of the granular material to be within ± 5 ° C., more preferably within ± 2 ° C., particularly preferably within ± 1 ° C.

  As a method for controlling the temperature change in this manner, (1) the amount and rate of addition of the anionic surfactant aqueous solution, (2) pressure in the granulator, (3) jacket temperature in the granulator, (4) Introducing air, inert gas and / or water vapor into the granulator, and (5) appropriately using one or two or more methods of appropriately adjusting the fluid number of the stirring blade of the granulator, etc. it can. Hereinafter, each method will be described in detail.

(1) Addition amount and addition rate of anionic surfactant aqueous solution It is preferable to control the addition amount and addition rate of the anionic surfactant aqueous solution so that the temperature of the granular material is within the above range. The added amount of the aqueous anionic surfactant solution is preferably such that the weight ratio of the aqueous anionic surfactant solution to the powder raw material is 1/10 to 10/1, and more preferably 4/4 to 7/1. As for the addition rate, it is difficult to obtain a granulated product if the time from the start of dropping the aqueous anionic surfactant solution until reaching the operating temperature is long, and if the dropping rate is too high, coarse particles may be obtained. It may become difficult to operate stably. For this reason, the ratio of the time required to reach the operating temperature and the addition time of the aqueous anionic surfactant solution is preferably 1/50 to 1/3.

(2) Pressure in the granulator The pressure in the granulator is preferably 40 kPa or less, more preferably 20 kPa or less, from the viewpoint of suppressing the decomposition of the aqueous solution and the granulated product by lowering the product temperature during operation. 0.0 kPa or less is particularly preferable. On the other hand, from the viewpoint of the burden on the vacuum pump and the airtightness of the granulator, 0.67 kPa or more is preferable, 1.5 kPa or more is more preferable, and 4.0 kPa or more is particularly preferable.

(3) Jacket temperature in the granulator The heating source of the granulator includes a warm water jacket, electric tracing, etc., but a warm water jacket is preferred, and the jacket temperature is preferably 100 ° C. or less, and is more sensitive to heat. 90 degreeC or less is still more preferable from a viewpoint of applying also to a raw material.

(4) Introduction of air, inert gas and / or water vapor into the granulator Air, inert gas and / or to the granulator in order to carry out drying more effectively during the addition of the aqueous anionic surfactant solution. Steam may be introduced. The introduction amount is preferably 2 to 30 L / min, more preferably 3 to 10 L / min.

(5) Froude number of agitation blade of granulator From the viewpoint of promoting compaction and sufficiently forming an adhesion layer to narrow the particle size distribution, the fluid number defined by the following formula is 1 to 5 Is more preferable, and 1.5 to 4 is more preferable.

Fr = V / [(R × g) ^0.5 ]
(Where Fr is the fluid number, V is the peripheral speed [m / sec.] Of the tip of the stirring blade, R is the rotation radius [m] of the stirring blade, and g is the acceleration of gravity [m / sec. ² ]. Showing).

  The granulator used in the present invention is preferably equipped with a stirring blade and a crushing blade and forms a clearance between the stirring blade and the wall surface when the stirring blade rotates. The average clearance is preferably 1 to 30 mm, more preferably 3 to 10 mm. When the average clearance is 1 mm or more, the pressure density of the adhesion layer is appropriate. Further, if the average clearance is 30 mm or less, the consolidation efficiency is good, the particle size distribution is not broad, and the productivity is good.

  Examples of the granulator preferably used in the present invention include, for example, a Henschel mixer (manufactured by Mitsui Miike Chemical Co., Ltd.), a high speed mixer (manufactured by Fukae Powtech Co., Ltd.), and a vertical granulator [(stock) ) Powrec], Redige mixer [Matsuzaka Giken Co., Ltd.], Pro-share mixer [Pacific Kiko Co., Ltd.], etc., particularly preferred Redige mixer [Matsuzaka Giken Co., Ltd.], high Speed mixer [Fukae Powtech Co., Ltd.], Pro-share mixer [Pacific Kiko Co., Ltd.]. Continuous type readyge mixer (medium speed mixer: relatively long residence time) as a continuous type, CB recycler (manufactured by Loedige) as a high speed mixer (relatively short residence time), turbulizer (Hosokawa Micron Co., Ltd.) Product), Shugi mixer (manufactured by POWREC Co., Ltd.), flow jet mixer (manufactured by Powder Research Co., Ltd.), and the like.

  Furthermore, the granulator used in the present invention is preferably equipped with a jacket for adjusting the internal temperature (article temperature) or equipped with a nozzle for performing a gas blowing operation. Specific examples of such a more preferred granulator include the granulators described in JP-A-10-296064, JP-A-10-296065, and Japanese Patent No. 3165700.

  In the present invention, when granulation is performed simultaneously with drying, it is preferable to carry out while blowing gas. This is in order to suppress the formation of a large lump of the granular material by evaporating water and cooling the obtained granular material using gas. Such gases include nitrogen gas, air, and / or water vapor.

  In the present invention, since the fine powder may remain after the addition of the aqueous anionic surfactant solution, it may have a step of rotating only the stirring blade without substantially rotating the crushing blade. It is preferable from the viewpoint of taking in (re-adhering fine powder to the powder).

[Method for producing high-purity anionic surfactant powder]
In the present invention, the crude anionic surfactant powder obtained as described above is first brought into contact with an extraction solvent for solid-liquid separation.

  In the present invention, the extraction solvent refers to a liquid that dissolves and disperses a part and all of the higher alcohol that is not sulfated and the by-produced hydrocarbon as referred to in the present invention.

  A general-purpose organic solvent can be used as the extraction solvent. The type is not particularly limited, but for example, aromatic hydrocarbons such as toluene and benzene, chlorinated aromatic hydrocarbons such as chlorobenzene, chlorinated aliphatic hydrocarbons such as dichloromethane and trichloromethane, methanol, ethanol, isopropyl Alcohols such as alcohol and butanol, esters such as ethyl acetate and butyl acetate, ethers such as tetrahydrofuran, isopropyl ether and diethyl ether, ketones such as acetone and methyl ethyl ketone, cellosolves such as methyl cellosolve, cyclohexane, methylcyclohexanol And alicyclic hydrocarbons such as normal hexane, isooctane, n-pentane, heptane and the like, and mixtures of the above solvents such as gasoline, petroleum ether and petroleum benzine. Of these, aromatic hydrocarbons, chlorinated aliphatic hydrocarbons, alcohols, ethers, ketones, aliphatic hydrocarbons, or mixtures thereof are preferably used. Isopropyl alcohol, toluene, normal hexane, acetone, and benzene are more preferable from the viewpoint of the price of the solvent and safety. From the viewpoint of extraction efficiency, petroleum ether, n-pentane, dichloromethane, diethyl ether, and tetrahydrofuran are more preferable.

  The extraction operation may be performed by a continuous operation, a batch operation, or a batch continuous operation. Examples of extractors that can be operated continuously include a Krupp extractor, Rotocel extractor, Kennedy extractor, Bollman extractor, Hildebrandt extractor, Bonotto extractor, Chiyoda L-type extractor, and pulse column. As an extractor capable of batch operation, there are a closed extraction tank and a pachuca tank. Moreover, as a batch continuous type extractor, there is a semi-continuous battery extraction device to which the Shanks method is applied.

  In the present invention, the temperature during the contact treatment of the crude anionic surfactant granules and the extraction solvent is preferably 70 ° C. or less, preferably 60 ° C. or less, from the viewpoint of suppressing thermal deterioration of the anionic surfactant granules. More preferred is 50 ° C. or less. Moreover, 10 degreeC or more is preferable, 20 degreeC or more is further more preferable, and 30 degreeC or more is especially preferable from a viewpoint of the solubility of the extract to an extraction solvent, and an extraction rate.

  In the solid-liquid extraction of the present invention, the weight ratio of the extraction solvent to the anionic surfactant powder is preferably 1/10 or more, more preferably 1/5 or more, and more preferably 3/10 or more from the viewpoint of productivity. Particularly preferred. Further, from the viewpoint of reducing consumption of the extraction solvent, 1/1 or less is preferable, 4/5 or less is more preferable, and 3/5 or less is particularly preferable. The used solvent can be reused, and it is preferable to distill to reduce the extract quality.

  In the production method of the present invention, since it is a solid-liquid extraction operation, it is possible to easily separate the treated anionic surfactant powder and extraction solvent. For example, in batch operation, separation can be easily performed by a perforated plate or a lattice-like net. Moreover, in the case of continuous operation, the anionic surfactant granular material processed with the screw, the blade | wing, the conveyor, etc. can be discharged | emitted.

  In the production method of the present invention, after separating the anionic surfactant granules from the extraction solvent, the extraction solvent and the like are removed by further drying the anionic surfactant granules. The drying temperature at this time is preferably 80 ° C. or lower, more preferably 70 ° C. or lower, and particularly preferably 60 ° C. or lower, from the viewpoint of preventing thermal deterioration of the anionic surfactant powder. Moreover, from a viewpoint of drying efficiency, 20 degreeC or more is preferable, 30 degreeC or more is more preferable, and 40 degreeC or more is especially preferable.

  The pressure at the time of drying is preferably atmospheric pressure or less, more preferably 40.0 kPa or less, particularly preferably 16.0 kPa or less, and most preferably 6.7 kPa or less from the viewpoint of thermal load reduction or drying efficiency.

[High purity anionic surfactant powder]
The high-purity anionic surfactant powder obtained by the production method of the present invention may further contain a water-soluble inorganic salt in addition to the anionic surfactant. Examples of the water-soluble inorganic salt include sodium chloride, sodium sulfate, sodium carbonate and the like. The content of the water-soluble inorganic salt in the anionic surfactant granules is not particularly limited, but from the viewpoint of keeping the solid content of the high-purity anionic surfactant granules high with respect to 100 parts by weight of the anionic surfactant 8 parts by weight or less, preferably 5 parts by weight or less, more preferably 2 parts by weight or less.

  The high-purity anionic surfactant granular material can contain a surfactant other than the anionic surfactant. Examples of the surfactant other than the anionic surfactant include a cationic surfactant and a nonionic surfactant.

  The high-purity anionic surfactant granular material can contain other additives as required. Examples of other additives include alkali agents such as silicates and carbonates, divalent metal ion scavengers such as citrate and zeolite, anti-contamination agents such as polyvinylpyrrolidone and carboxymethylcellulose, and other anti-caking agents. And antioxidants. Such other additives can be used as long as the object of the present invention is not impaired.

  The unreacted material contained in the high-purity anionic surfactant powder is not preferable because it causes a decrease in purity and caking properties of the powder, but it is acceptable if it is 1% by weight or less, More preferably, it is 0.8 weight% or less, More preferably, it is 0.5 weight% or less. Here, the unreacted material includes higher alcohols and alkoxylates that have not been sulfated, and a small amount of hydrocarbons and wax by-produced from the reaction. The amount of unreacted substances was determined according to a method for determining petroleum ether-soluble matter (JIS K 3362).

  The shape of the high-purity anionic surfactant powder is not particularly limited, and examples thereof include powder, needle, flake, noodle, granule, pellet, and tablet. Furthermore, you may grind | pulverize or process the obtained high purity anionic surfactant granular material. Of these, granules and pellets are preferred from the viewpoint of ease of handling and ease of dispersion / dissolution during use.

  The average particle diameter of the high-purity anionic surfactant powder is preferably 0.1 mm or more, more preferably 0.2 mm or more, and more preferably 0.5 mm or more from the viewpoint of ease of handling and solid-liquid separation. Is particularly preferred. Moreover, 3 mm or less is preferable from a viewpoint of solubility or caking resistance, 2 mm or less is further more preferable, and 1.5 mm or less is especially preferable. In addition, the average particle diameter in this invention is measured from the weight fraction by the size of the mesh after vibrating for 5 minutes using the standard sieve of JISZ8801.

The bulk density of the high-purity anionic surfactant powder, from the viewpoint of charging efficiency, preferably 400 kg / m ³ or more, more preferably 500 kg / m ³ or more, 600 kg / m ³ or more is particularly preferable. From the viewpoint of ease of production, it is preferably 1000 kg / m ³ or less, more preferably 900 kg / m ³ or less. The bulk density in the present invention is a value determined by a method defined in JIS K 3362.

  The water content of the high-purity anionic surfactant powder is preferably 3% by weight or less, more preferably 2.5% by weight or less, and particularly preferably 2.0% by weight or less from the viewpoint of caking resistance. Moreover, 0.3 weight% or more is preferable from a viewpoint of reducing the dust generation by the contact between granular materials, 0.5 weight% or more is further more preferable, and 1.0 weight% or more is especially preferable. The water content of the granular material is measured by a method such as a heat loss method, a distillation method, or a Karl Fischer method (JIS K 0068). The water content in this specification was measured by the Karl Fischer method (JIS K 0068). Value.

  From the viewpoint of effectively exhibiting the function of the anionic surfactant itself, the high-purity anionic surfactant powder is 90% by weight or more of the anionic surfactant, preferably 95% by weight or more, and more preferably 95% by weight or more. Preferably it contains 98 weight% or more. The anionic surfactant content is measured by the Epton method (JIS K 3362).

  From the viewpoint of handling, the fluidity is preferably 10 seconds or less, and more preferably 8 seconds or less. The fluidity of the high-purity anionic surfactant granular material in the present invention is the time required for 100 mL of granular material to flow out from the hopper for measuring bulk density specified in JIS K 3362.

  From the viewpoint of enhancing the quality and value of commercial products and blended products, APHA is preferably 30 or less, more preferably 20 or less, and particularly preferably 10 or less. Further, from the viewpoint of ease of production, APHA is preferably 3 or more, more preferably 5 or more, and particularly preferably 10 or more. The hue is measured by a method of JIS K0071 using a 10% by weight aqueous solution of an anionic surfactant granular material.

As the high purity anionic surfactant powder particles of the present invention, those satisfying all the following conditions (A) to (E) are particularly preferable.
(A) Unreacted material amount: 1.0% by weight or less (B) Average particle size: 0.1 to 3.0 mm
(C) Bulk density: 400 to 1000 kg / m ³
(D) Color: APHA 3-30
(E) Anionic surfactant content: 90% by weight or more.

  In the present invention, efficient solvent extraction is possible in the state of the granular material, regardless of the production method for obtaining the crude anionic surfactant granular material. In addition, the use of a crude anionic surfactant powder obtained by a method of simultaneously granulating and drying from an aqueous anionic surfactant solution is preferable because of high solvent extraction efficiency despite its denseness. This is presumed to be because the extraction solvent between the particles is efficiently replaced due to the high uniformity of the particle size and shape. Further, even when the crude anionic surfactant powder particles are pulverized, it is possible to remove sufficient impurities, which is presumed to be caused by an increase in specific surface area.

  In the examples, “%” means “% by weight” unless otherwise specified.

Synthesis example 1
In a thin film flow-down reactor having an inner diameter of 16 mmφ and a length of 5 m, together with 2.0% by volume of sulfur trioxide gas, the alkyl group has 12 to 16 carbon atoms and its distribution is C ₁₂ / C ₁₄ / C ₁₆ = 67% A higher alcohol (molecular weight: 199) of / 28% / 5% was continuously added at 60 ° C. for reaction. The flow rate was adjusted so that the reaction molar ratio of sulfur trioxide gas to higher alcohol was 1.01. The obtained sulfate was neutralized with a 32.2% sodium hydroxide aqueous solution, 75% phosphoric acid (buffer) was added, and then finely adjusted to pH = 10 with a 32.1% sodium hydroxide aqueous solution. The water content was adjusted to 24% to obtain an aqueous sodium alkylsulfate salt solution (hereinafter referred to as an anionic surfactant aqueous solution 1).

Synthesis example 2
4.3 kg of alkyl sulfate sodium salt powder [EMAL 10P-HD: manufactured by Kao Corporation, average particle size 100 μm] is put into a vacuum dryer having a capacity of 65 L [FMD-65JE type, manufactured by Fukae Pautech Co., Ltd.] Anionic surfactant obtained in Synthesis Example 1 under dry granulation conditions of jacket temperature 85 ° C., pressure in granulator: 6.7 kPa, agitator rotation speed: 200 r / min, chopper rotation speed: 3000 r / min After dripping the aqueous solution 1 into the dryer at an addition rate of 19.7 kg / hr, the dripping flow rate of the anionic surfactant aqueous solution 1 is adjusted so that the product temperature becomes 60 ± 2 ° C. Done the grain. Thereafter, when the total amount of the anionic surfactant aqueous solution 1 dropped to 20 kg, the dry granulation was completed, the average particle size: 800 μm, the bulk density 706 kg / m ³ , the anionic surfactant content: 97.1%, the moisture A granulated product of alkyl sulfate sodium salt [average molecular weight: 301] having a content of 1.4% and an unreacted content of 1.3% was obtained. This was classified with a sieve having an opening of 1000 μm and 1180 μm to obtain 5 kg of sodium alkyl sulfate salt powder (hereinafter referred to as anionic surfactant powder 1) having a particle size of 1000 to 1180 μm.

Example 1
2 g of the anionic surfactant powder 1 obtained in Synthesis Example 2 was weighed into a sealed glass container with a 20 mL capacity lid, and then 10 mL of acetone as an extraction solvent was injected, and the lid was closed. A temperature controller (EYELA T-80 manufactured by Tokyo Rika Kikai Co., Ltd.) was attached to a water bath filled with water (EYELA SB-24 manufactured by Tokyo Rika Kikai Co., Ltd.) and adjusted to 40 ° C. in advance. The glass container containing activator powder 1 and acetone was immersed and extracted by shaking for 10 minutes with a shaker (EYELA SS-8, manufactured by Tokyo Rika Kikai Co., Ltd.). Thereafter, the anionic surfactant granular material extracted from the glass container and acetone were taken out on a wire mesh of 75 μm (200 mesh) and filtered. Next, the separated anionic surfactant powder on the wire mesh is put into a vacuum constant temperature dryer (DP43 model, manufactured by Yamato Scientific Co., Ltd.), dried at a temperature of 40 ° C. and a pressure of 4.0 kPa for 15 minutes, and then taken out. A high-purity anionic surfactant powder having a reaction content reduced to 0.95% was obtained. Table 1 shows the amount of unreacted substances in the obtained high-purity anionic surfactant powder.

Examples 2-8
A high-purity anionic surfactant granular material was obtained in the same manner as in Example 1 except that the amount of the anionic surfactant granular material 1, the extraction solvent and the extraction conditions were changed as shown in Table 1. Table 1 shows the amount of unreacted substances in the obtained high-purity anionic surfactant powder.

Comparative Example 1
The anionic surfactant aqueous solution 1 obtained in Synthesis Example 1 was charged into a 2 L Separa flask and stirred while being kept at 60 ° C. in a water bath. Next, 200 mL of normal hexane was added while maintaining the temperature at 60 ° C. The mixture of the anionic surfactant aqueous solution 1 and normal hexane gelled. This was centrifuged with a centrifugal separator (XX42 CF0 0T type, manufactured by Tokyo Glass Instruments Co., Ltd.), and the precipitated anionic surfactant aqueous solution was transferred to a petri dish and placed in a vacuum constant temperature dryer (DP43 type, manufactured by Yamato Scientific Co., Ltd.). After drying all day and night at 40 ° C. and a pressure of 4.0 kPa, it was taken out and crushed. The unreacted material of the anionic surfactant powder was 1.22%.

Comparative Example 2
The anionic surfactant powder 1 obtained in Synthesis Example 2 was not extracted with a solvent, but placed in a vacuum constant temperature dryer (DP43 model, manufactured by Yamato Scientific Co., Ltd.) at a temperature of 40 ° C. and a pressure of 4.0 kPa. Dry for 15 minutes. The unreacted substance of the obtained anionic surfactant powder was 1.29%.

Claims (6)

  Contains 90% by weight or more of the anionic surfactant obtained by subjecting the crude anionic surfactant granules to contact with the extraction solvent, separating the anionic surfactant granules from the extraction solvent, and drying. To produce a high-purity anionic surfactant powder.   The production method according to claim 1, wherein the contact treatment is carried out by immersing the crude anionic surfactant powder particles in an extraction solvent at a temperature of 10 to 70 ° C.   The manufacturing method of Claim 1 or 2 which performs drying at the temperature of 20-80 degreeC.   The production method according to any one of claims 1 to 3, wherein the crude anionic surfactant granular material is obtained by a method of simultaneously performing drying and granulation.   The production method according to any one of claims 1 to 4, wherein the average particle diameter of the crude anionic surfactant powder is 0.1 to 3 mm. The production method according to claim 1, wherein the crude anionic surfactant powder has a bulk density of 400 to 1000 kg / m ³ .