Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for removing floc in bis(2-mercaptoethyl)sulfide and improving product purity and yield

A dimercaptoethyl sulfide, flocculent technology, applied in sulfide preparation, organic chemistry and other directions, can solve the problems of low product purity, betting tower, low product yield and so on

Inactive Publication Date: 2019-04-19
锦西化工研究院有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is simple, but there are flocs in the product, the product is low in purity, and the product is not clear; and due to the presence of flocs, in the subsequent vacuum distillation process, there is a betting tower phenomenon, industrial operation is difficult, and the product yield is low. Low
Hubei Huida Science and Technology Development Co., Ltd. Ling Yun et al. used thiodiglycol and thiourea to generate sulfonium urea salts, and synthesized dimercaptoethyl sulfide through alkaline hydrolysis, but added catalysts, phase transfer catalysts, and antioxidants during the reaction process. Agents and other substances, there are many raw materials, long reaction time, easy decomposition of products and other problems

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for removing floc in bis(2-mercaptoethyl)sulfide and improving product purity and yield
  • Method for removing floc in bis(2-mercaptoethyl)sulfide and improving product purity and yield

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add the dimercaptoethyl sulfide reaction solution (I) to a 500L reactor equipped with a stirrer, a thermometer and a reflux condenser, add concentrated hydrochloric acid to a pH of 5, and after reacting at room temperature for 1 hour, stop stirring. Stand still for 1 hour, and then separate in a specific reactor to retain the lower layer liquid; pass water into the lower mouth of the reactor so that the water flows naturally from the bottom up from the upper mouth, fully contact with the material, and remove the remaining floccules in the reaction liquid. The material is brought to the upper layer of the product, and after the water is washed to neutrality, the lower product, namely the crude dimercaptoethyl sulfide (II), is released to realize the continuous operation of the water washing process. Under reduced pressure distillation, a colorless and transparent dimercaptoethyl sulfide product was obtained. The purity is 99.3%, and the yield is 91.8%.

Embodiment 2

[0023] Add the dimercaptoethyl sulfide reaction solution (I) to a 500L reactor equipped with a stirrer, a thermometer, and a reflux condenser, add concentrated hydrochloric acid to a pH of 3, and after reacting at room temperature for 1 hour, stop stirring. Stand still for 1 hour, and then separate in a specific reactor to retain the lower layer liquid; pass water into the lower mouth of the reactor so that the water flows naturally from the bottom up from the upper mouth, fully contact with the material, and remove the remaining floccules in the reaction liquid. The material is brought to the upper layer of the product, and after the water is washed to neutrality, the lower product, namely the crude dimercaptoethyl sulfide (II), is released to realize the continuous operation of the water washing process. Under reduced pressure distillation, a colorless and transparent dimercaptoethyl sulfide product was obtained. The purity is 98.4%, and the yield is 89.1%.

Embodiment 3

[0025] Add the dimercaptoethyl sulfide reaction solution (I) to a 500L reactor equipped with a stirrer, a thermometer and a reflux condenser, add concentrated hydrochloric acid to a pH of 6, and react at room temperature for 1 hour, then stop stirring. Stand still for 1 hour, and then separate in a specific reactor to retain the lower layer liquid; pass water into the lower mouth of the reactor so that the water flows naturally from the bottom up from the upper mouth, fully contact with the material, and remove the remaining floccules in the reaction liquid. The material is brought to the upper layer of the product, and after the water is washed to neutrality, the lower product, namely the crude dimercaptoethyl sulfide (II), is released to realize the continuous operation of the water washing process. Under reduced pressure distillation, a colorless and transparent dimercaptoethyl sulfide product was obtained. The purity is 98.4%, and the yield is 90.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention aims to develop a method for removing aminohydrogen floc in a bis(2-mercaptoethyl)sulfide product and improving product purity and yield. In the synthetic process of bis(2-mercaptoethyl)sulfide, the acidifying process is additionally arranged, and aminohydrogen is converted to salt through an addition reaction between hydrochloric acid and aminohydrogen; and then through separation,washing, separation and rectification, the product is obtained. Through the design of reasonable washing and separation equipment, continuous washing process is realized, working environment is improved, and labor intensity is reduced; and the tower blocking problem of floc in the subsequent distillation process is solved. The process has the following advantages: the production process is stablein operation, and industrial production is realized; appearance of the product is improved, the product is clear and transparent, and the product purity is increased from 95% to 99% and above; and theyield is increased from 75% to 90% and above.

Description

Technical field [0001] The invention belongs to the technical field of organic chemical production, and specifically relates to an industrial synthesis method and post-treatment operation process of dimercaptoethyl sulfide. Background technique [0002] With the development of my country's aviation industry, especially the development of new models, higher requirements are put forward for the adhesion, aging resistance, and stability of sealing materials. Polysulfide rubber with traditional polysulfide rubber as the main agent The sealant can no longer meet the requirements. The viscosity of polysulfide rubber modified by dimercaptoethyl sulfide is significantly lower than that of traditional liquid polysulfide rubber, which can better match fillers, reduce costs, and at the same time improve the aging resistance of the material and the use temperature of the material It is -55℃~120℃, can reach 150℃ in the short term, and has the characteristics of oil resistance, water resistanc...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/20C07C321/14
CPCC07C319/20C07C335/32C07C321/14
Inventor 赫平李锦马天野李放王迪
Owner 锦西化工研究院有限公司