CN-122010793-A - Preparation method of fatty alcohol sulfoacetate sodium salt

Abstract

The invention discloses a preparation method of fatty alcohol sulfoacetate sodium salt, and relates to the technical field of chemical synthesis. The method is mainly used for synthesizing the sodium fatty alcohol sulfoacetate by adopting a mechanical method, has the advantages of low reaction temperature, high conversion rate, no gel phenomenon in the reaction process, few byproducts, low production cost, light color, small smell and good stability, and can be better applied to the daily chemical field.

Inventors

• XIE ZHIKAI
• LIU ZHENHUA
• YANG WENLING
• ZHANG YONG
• CHEN SHENGHUAN
• HU WENJIE

Assignees

• 广州花语精细化工有限公司

Dates

Publication Date

20260512

Application Date

20260115

Claims (10)

1. 1. The preparation method of the fatty alcohol sulfoacetate sodium salt is characterized by comprising the following steps of: (1) Adding fatty alcohol and chloroacetic acid into a flask, heating and dissolving, adding a catalyst, heating and preserving heat for reaction, and cooling to obtain a crude product of fatty alcohol chloroacetate; (2) Placing the crude product of the fatty alcohol chloroacetate in a separating funnel, recovering the catalyst at the lower layer, washing the upper layer solution with water, and separating the upper layer solution to obtain the fatty alcohol chloroacetate; (3) Adding fatty alcohol chloroacetate into a ball milling tank, adding a sulfonating agent and a ball milling medium for grinding to obtain fatty alcohol sulfoacetate sodium salt.
2. 2. The method for producing a sodium salt of aliphatic alcohol sulfoacetate according to claim 1 wherein said step (1) comprises at least one of the following (a) to (f): (a) The fatty alcohol comprises a single higher alcohol or a mixed higher alcohol; (b) The carbon number of the fatty alcohol is 8-20; (c) The mol ratio of the fatty alcohol to the chloroacetic acid is fatty alcohol chloroacetic acid=1:0.8-2.0; (d) The catalyst is an acid catalyst; (e) The dosage of the catalyst is 1.0-5.0% of the mass of fatty alcohol; (f) The heating and heat preserving reaction is specifically heating to 100-150 ℃, preserving heat until no water is distilled out, and then continuing the reaction for 0-3h.
3. 3. The method for producing sodium salt of fatty alcohol sulfoacetate according to claim 1 wherein the amount of water added in said step (2) is 10 to 50% by mass of fatty alcohol chloroacetate.
4. 4. The method for producing a sodium salt of aliphatic alcohol sulfoacetate according to claim 1 wherein the number of washing in said step (2) is 0 to 5.
5. 5. The method for producing a sodium salt of aliphatic alcohol sulfoacetate according to claim 1 wherein said step (3) comprises at least one of the following (a) to (c): (a) The sulfonating agent comprises at least one of concentrated sulfuric acid, chlorosulfonic acid, sulfur trioxide, sodium sulfite or sodium bisulfite; (b) The ball milling medium comprises at least one of stainless steel, zirconia, tungsten carbide or alumina; (c) The specific parameters of grinding are frequency of 15-45Hz, temperature of 30-80 ℃ and time of 0-4h.
6. 6. The method for producing sodium salt of aliphatic alcohol sulfoacetate according to claim 5 wherein said sulfonating agent in step (3) is a mixture of sodium sulfite and sodium bisulfite.
7. 7. The method for producing sodium salt of aliphatic alcohol sulfoacetate according to claim 6 wherein the molar ratio of sodium sulfite to sodium bisulfite in said sulfonating agent is 5.66-19:1.
8. 8. The method for preparing sodium salt of aliphatic alcohol sulfoacetate according to claim 5 wherein said ball milling medium is 6-10 mm zirconia or alumina.
9. 9. The method for preparing sodium salt of aliphatic alcohol sulfoacetate according to claim 5 wherein the specific parameters of said grinding are frequency of 30-35Hz, temperature of 40-60 ℃ and time of 1-2h.
10. 10. Use of the process for the preparation of fatty alcohol sulfoacetate sodium salt according to any of claims 1 to 9 in the production of anionic surfactants.

Description

Preparation method of fatty alcohol sulfoacetate sodium salt Technical Field The invention relates to the technical field of chemical synthesis, in particular to a preparation method of fatty alcohol sulfoacetate sodium salt. Background Fatty alcohol sulfoacetate sodium salt is used as a mild anionic surfactant, and is widely applied in the field of high-end personal care, such as bath foam, shampoo, face cleaning product, bubble bath ball and the like, due to the good foam property, low irritation and natural biodegradability of the fatty alcohol sulfoacetate sodium salt. Compared with K12 (sodium dodecyl sulfate) and AES (sodium fatty alcohol polyoxyethylene ether sulfate), the detergent is milder and can be used in infant washing products. In addition, the fatty alcohol sulfoacetate sodium salt has the anti-inflammatory and bactericidal effects, so that the fatty alcohol sulfoacetate sodium salt also serves as a pharmaceutical auxiliary material and plays a role in the fields of dental care products, intestine-moistening medicines and the like. At present, few reports are about the synthesis of fatty alcohol sodium sulfoacetate, and the synthesis is mainly divided into two synthetic ideas, namely esterification and sulfonation and direct esterification. Chinese patent CN109293533A is prepared by esterifying lauryl alcohol and acetic acid to form laurylacetate, sulfonating the laurylacetate sodium by using sodium methane sulfonate as sulfonating agent, wherein Chinese patent CN109796378A is prepared by directly esterifying sodium sulfoacetate and fatty alcohol to obtain fatty alcohol sodium sulfoacetate, and is reported to be sulfonated with excessive sodium sulfite after esterification of bromoacetic acid fatty alcohol, and earlier, chloroacetyl chloride and fatty alcohol are also adopted to be esterified and then sulfonated. However, whether it is esterified first and then sulphonated or directly esterified, high temperature heating is required during the reaction, since the melting point of the product is above 150 ℃, and the thickening of the material in water is strong, and a 20% aqueous solution is in an insoluble state. Therefore, the product is generally sold as powder in the market, and there is a large market mainly in europe, the united states, canada, korea and japan, australia, southeast asia countries, etc., but the product is still under exploration in China. Disclosure of Invention The invention aims to overcome the defects of the prior art and provides a preparation method of fatty alcohol sulfoacetate sodium salt. In order to achieve the aim, the technical scheme adopted by the invention is that the preparation method of the fatty alcohol sulfoacetate sodium salt comprises the following steps: (1) Adding fatty alcohol and chloroacetic acid into a flask, heating and dissolving, adding a catalyst, heating and preserving heat for reaction, and cooling to obtain a crude product of fatty alcohol chloroacetate; (2) Placing the crude product of the fatty alcohol chloroacetate in a separating funnel, recovering the catalyst at the lower layer, washing the upper layer solution with water, and separating the upper layer solution to obtain the fatty alcohol chloroacetate; (3) Adding fatty alcohol chloroacetate into a ball milling tank, adding a sulfonating agent and a ball milling medium for grinding to obtain fatty alcohol sulfoacetate sodium salt. The existing method for preparing the sodium fatty alcohol sulfoacetate has the disadvantages of low purity, more byproducts, high reaction temperature, gel-like state in the reaction process, difficult stirring, mass transfer influence, energy consumption problem for later water removal due to the addition of a large amount of water, and high discharge temperature which is required to be above 150 ℃. In addition, since the ester is insoluble in water, a phase transfer catalyst is often required to be added in the reaction process to improve the reaction yield, and the pH of the aqueous solution of sodium sulfite is about 9, so that the unreacted ester is inevitably hydrolyzed into corresponding fatty alcohol at high temperature along with the increase of temperature, thereby reducing the conversion rate of the reaction. The preparation method of the sodium fatty alcohol sulfoacetate salt aims at solving the problems that the sulfonation reaction temperature is high, sticky agglomeration occurs in the reaction process of the product, mass transfer is poor, a phase transfer catalyst is used and sodium sulfite aqueous solution easily causes ester hydrolysis, and the sodium fatty alcohol sulfoacetate salt is synthesized by adopting a mechanical method without a solvent, so that the stirring difficulty caused by thickening in the reaction process is solved, the mass transfer efficiency of materials is improved, the use of solvents is avoided, the water removal problem of subsequent powder formation is reduced, the post-treatment steps are reduced, the cost