Production method of high-purity 3-chloro-1, 2-propanediol

Abstract

The invention discloses a production method of high-purity 3-chloro-1, 2-propanediol, which comprises the following steps: (1) taking sulfuric acid, benzenesulfonic acid and succinic acid, respectively dissolving the three in deionized water, and preparing into sulfuric acid solution, benzenesulfonic acid solution and succinic acid solution; (2) firstly mixing part of the sulfuric acid solution, part of the benzenesulfonic acid solution and part of epichlorohydrin, carrying out reaction for a period of time, raising temperature, further adding the remaining epichlorohydrin, sequentially adding the remaining benzenesulfonic acid solution and the sulfuric acid solution according to time periods, then adding the succinic acid solution once, raising the temperature, and continuously carrying out the reaction; (3) adding alkaline solution after completing hydrolysis reaction, and stirring for leading the reaction to be uniform; (4) carrying out dehydration on hydrolysate after adding the alkaline solution, adding the alkaline solution after finishing the dehydration, and raising the temperature under stirring condition; and (5) firstly heating materials under vacuum condition, then transferring the materials into a distillation system, and obtaining a product of 3-chloro-1, 2-propanediol by distillation when the vacuum degree is not less than 0.1MPa.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a production method of high-purity 3-chloro-1,2-propanediol. Background technique [0002] 3-Chloro-1,2-propanediol (referred to as chloroglycerin) is an important chlorinated glycerol with a wide range of uses: it can be used as an intermediate in organic synthesis to synthesize pesticides, dyes, medicines, paints, veterinary drugs, plasticizers, surface Active agent and printing and dyeing auxiliary agent, etc.; can be used as a solvent for the production of cellulose acetate, etc.; can also be used as an important reagent in medical research, used in the research of reproductive medicine; in the past ten years, in aerospace materials, non-ionic imaging The application of chemical reagents, electronic chemicals, catalyst synthesis, and phase transfer catalyst applications is becoming more and more extensive, and the requirements for the purity and impurity content of chlorogly...

AI Technical Summary

Problems solved by technology

However, during the production of epichlorohydrin method, due to the influence of catalyst selection, use, feeding sequence, gradient temperature rise and other technical aspects, especially the influence of factors such as equipment selection and process conditions in the final distillation process, the purity of the obtained product is general. Less than 99.5% (GC), there are also problems such as improving the purity that will lead to a decline in yield, which directly affects the economic benefits and market competition of the product

Although some domestic enterprises have adopted the vacuum scraper thin film evaporation method for the separation of chloroglycerin, the problems of high purity and high impurity peak after the main peak of chromatographic analysis and high impurity content have not been solved.