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

A production method and high-purity technology, applied in the field of high-purity 3-chloro-1, can solve problems such as yield decline, impact on product economic benefits and market competition, and less than 99.5%, and achieve shortened hydrolysis reaction period and product quality. Stable, extended shelf life effect

Inactive Publication Date: 2010-12-29
青岛中科荣达新材料有限公司
View PDF1 Cites 13 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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 improvin

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Ingredients: Dissolve 1.15Kg of industrial sulfuric acid, 0.6Kg of benzenesulfonic acid and 0.25Kg of succinic acid in 280Kg, 190Kg and 130Kg of deionized water respectively; measure 300Kg of epichlorohydrin for later use.

[0031] 2. Hydrolysis reaction: The reaction is carried out in a 1000L enamel kettle. Add 140Kg of sulfuric acid solution and 100Kg of benzenesulfonic acid solution into the hydrolysis tank first, and the remaining sulfuric acid solution and benzenesulfonic acid solution are pumped into the high level tank respectively. Add 200Kg epichlorohydrin into the hydrolysis tank, react at 72°C for 60 minutes, raise the temperature to 88°C, add the remaining epichlorohydrin at one time, and then add the remaining benzenesulfonate dropwise within 20 to 30 minutes Acid solution, then add the remaining sulfuric acid solution dropwise within 30-45 minutes. After the dropwise addition, add the succinic acid solution into the hydrolysis kettle at one time, raise ...

Embodiment 2

[0039] 1. Ingredients: Dissolve 2.4Kg of industrial sulfuric acid, 1.3Kg of benzenesulfonic acid and 0.55Kg of succinic acid in 580Kg, 410Kg and 290Kg of deionized water respectively; measure 650Kg of epichlorohydrin for later use.

[0040] 2. Hydrolysis reaction: The reaction is carried out in a 2000L enamel kettle. Add 300Kg of sulfuric acid solution and 210Kg of benzenesulfonic acid solution into the hydrolysis tank first, and the remaining sulfuric acid solution and benzenesulfonic acid solution are pumped into the high level tank respectively. Add 450Kg of epichlorohydrin into the hydrolysis tank, react at a temperature of 74°C for 65 minutes, raise the temperature to 85°C, add the remaining epichlorohydrin at one time, and add the remaining benzenesulfonate dropwise within 20 to 30 minutes Acid solution, then add the remaining sulfuric acid solution dropwise within 30-45 minutes. After the dropwise addition, add the succinic acid solution into the hydrolysis kettle at on...

Embodiment 3

[0048] 1. Ingredients: Dissolve 2.35Kg of industrial sulfuric acid, 1.4Kg of benzenesulfonic acid and 0.45Kg of succinic acid in 570Kg, 400Kg and 250Kg of deionized water respectively; measure 600Kg of epichlorohydrin for later use.

[0049] 2. Hydrolysis reaction: The reaction is carried out in a 2000L enamel kettle. Put 290Kg sulfuric acid solution and 200Kg benzenesulfonic acid solution into the hydrolysis tank first, and the remaining sulfuric acid solution and benzenesulfonic acid solution are pumped into the high level tank respectively. Add 400Kg of epichlorohydrin to the hydrolysis tank, react at a temperature of 75°C for 70 minutes, raise the temperature to 84°C, add the remaining epichlorohydrin at one time, and then add the remaining benzenesulfonate dropwise within 20 to 30 minutes Acid solution, then add the remaining sulfuric acid solution dropwise within 30-45 minutes. After the dropwise addition, add the succinic acid solution into the hydrolysis kettle at one ...

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 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...

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
IPC IPC(8): C07C31/42C07C29/10C07C29/80
Inventor 张中法郭学阳丁爱梅黄慧吕彩玲张庆国魏丽华
Owner 青岛中科荣达新材料有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap