JPH0640947B2 - Method for producing low-moisture, high-concentration anionic surfactant - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a low water content and high concentration anionic surfactant.

Sodium and potassium salts of sulfuric acid esters of higher alcohols, alkylphenols, alkylene oxide adducts of higher alcohols or alkylphenols are currently produced in large quantities and are used as detergents, emulsifiers, dispersants, etc. Are commercially available as low-moisture powder products in the form of an aqueous solution or paste contained in, or a large amount of an inorganic salt such as mirabilite, sodium tripolyphosphate, or soda ash, which is then dried and then dried. .

However, since it contains a large amount of water and a large amount of an inorganic salt, its use may be limited. Examples thereof include solvent-based dispersants, detergents, emulsifiers, emulsifiers for agricultural chemicals that are easily decomposed into water, dispersants, antistatic agents that are kneaded into plastics, water repellent additives, and oil-based lubricants. To be

The present inventors have arrived at the present invention as a result of earnest research in order to solve such problems. That is, the present invention is a step of sulfating a compound having at least one hydroxyl group in the molecule, and / or a neutralization step of forming an alkali metal salt, in the presence of water, a low boiling point solvent and the low boiling point solvent The present invention provides a method for producing a low-moisture, high-concentration anionic surfactant, which is characterized by blending a high-boiling point solvent which does not undergo azeotropic distillation.

In the present invention, as a compound having at least one hydroxyl group in the molecule, alkyl or aralkylphenol such as nonylphenol, dodecylphenol, distyrenated phenol and tribenzylphenol, higher alcohol such as lauryl alcohol, stearyl alcohol and oleyl alcohol, glycerin , Sucrose,
Examples thereof include polyhydric alcohols such as polyethylene glycol and polypropylene glycol, and alkylene oxide (ethylene oxide, propylene oxide, styrene oxide) adducts of the above-mentioned alkylphenols, higher alcohols, polyhydric alcohols such as glycerin and sucrose.

The sulfating agent includes sulfuric acid, fuming sulfuric acid, chlorosulfonic acid, sulfuric anhydride, and sulfamic acid. However, with sulfamic acid, an ammonium salt can be obtained and sodium substitution may be possible, but there are many problems such as an increase in the number of steps and generation of ammonium odor, which is not preferable in the present invention.

In the neutralization step of the present invention, sodium hydroxide, potassium hydroxide, sodium ethoxide, potassium ethoxide, sodium methoxide and potassium methoxide are used. Although it has a drawback that water is generated during neutralization, sodium hydroxide and potassium hydroxide are preferable from the viewpoint of inexpensiveness.

Further, in the present invention, the low boiling point solvent means acetone, chloroform, methanol, 1,1,1, which has a lower boiling point than water.
-Trichloroethane, carbon tetrachloride, ethanol, methyl ethyl ketone, benzene, isopropyl alcohol and the like, but methanol and ethanol, which are inexpensive and easily form methoxide and ethoxide, are more preferable.

Further, in the present invention, the high boiling point solvent which does not azeotrope with the low boiling point solvent is decompressed at 70 to 100 ° C. (15 to 30 mmH).
g) Water and a solvent that does not azeotrope with the low boiling point solvent during dehydration and solvent removal, such as distyrenated phenol, tristyrenated phenol, tribenzylphenol, benzyl alcohol, methylpyrrolidone,
Examples thereof include quinoline, ethylene carbonate, diethylene glycol, glycerin, and high-boiling isoparaffin (150 ° C or higher).

The present invention will be specifically described with reference to examples, but the present invention is not limited thereto.

Example 1 In a separable flask of 11, distyrenated phenol 3 was added.
00g and odorless isoparaffin (Nisseki Isozol 300
60 g (boiling point 170 ° C.), and 100 g of chlorsulfonic acid is added dropwise in a temperature range of 15 to 25 ° C. while stirring in a nitrogen stream.

After completion of the reaction, the above sulfated product is dropped into another 21-separable flask (40 g of flake caustic soda is dissolved in 500 g of methanol in advance) while being carefully added so that the temperature does not exceed 40 ° C. to neutralize. After leaving the neutralized solution overnight, the salt was removed by filtration, and the filtrate was evaporated (80
Methanol) and water are completely removed by (.degree. C.).
Then, when the obtained sulfuric acid ester / sodium salt of distyrenated phenol is analyzed, the water content (Karl Fischer method) is 1.5% and the viscosity (B type viscometer, at 20 ° C.) 56
It was 00 cps.

Example 2 300 g of a synthetic higher secondary alcohol (having 12 to 14 carbon atoms) was placed in a separable flask of 11, and the mixture was placed in a nitrogen stream,
While stirring, 110 g of chlorosulfonic acid was added to 15-25
Dropwise in the temperature range of ° C. After completion of the reaction, neutralization is carried out in another 21 separable flask (previously dissolved 62 g of caustic potash in a mixed solvent of 550 g of methanol and 30030 g of Isozole) so that the temperature of the sulfated product does not exceed 40 ° C.

Thereafter, the same procedure as in Example 1 was carried out to obtain the obtained synthetic high-grade second material.
As a result of analysis of sulfate / potassium salt of primary alcohol, water content 0.5%, viscosity (B type viscometer, at 20 ° C.) 1
It was 450 cps.

Example 3 A separable flask of 11 was charged with 680 g of an ethylene oxide 10 mol adduct of a synthetic higher secondary alcohol (the same as in Example 2) and 70 g of odorless isoparaffin (Nisseki Isozol 400 boiling point 206 ° C.) in a nitrogen stream. While stirring, 120 g of chlorosulfonic acid at 15 to 25 ° C
In the temperature range of.

After completion of the reaction, the above sulfated product is added dropwise to another 21 separable flask (43 g of caustic soda is dissolved in 700 g of ethanol in advance) at 40 ° C. or lower to neutralize.

Thereafter, the same procedure as in Example 1 was carried out to obtain the obtained synthetic high-grade second material.
When the sulfuric acid ester sodium salt of an ethylene oxide adduct of a primary alcohol was analyzed, the water content was 0.8% and the viscosity was 4300 cps (B-type viscometer, at 20 ° C.).

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Claims (1)

[Claims] 1. A low-boiling solvent and a low-boiling solvent in the presence of water in the step of sulfating a compound having at least one hydroxyl group in the molecule and / or the step of neutralizing an alkali metal salt. A method for producing an anionic surfactant having a low water content and a high concentration, which comprises blending a high boiling point solvent which does not boil.