Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of cyanoacetic acid and derivatives thereof

A technology of cyanoacetic acid and sodium cyanoacetate, applied in the field of preparation of cyanoacetic acid and derivatives thereof, can solve the problems of complicated operation, high cost, large amount of organic solvent, etc., and achieves simple operation, low production cost, and less amount of three wastes. Effect

Active Publication Date: 2016-02-03
CHONGQING UNISPLENDOUR CHEM
View PDF9 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of organic solvent used is large (the ratio of solvent to mixed solution is 1-5:1), the number of extractions is 4-8 times, the operation is cumbersome and the cost is high

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
  • Preparation method of cyanoacetic acid and derivatives thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] refer to figure 1 , the present invention is further described:

[0026] (1) Cyanide reaction: 96.8g of chloroacetic acid (content 98%, 1.0mol) and 70g of water were stirred and dissolved, and neutralized to pH=6.5-7.0 with 25% aqueous sodium carbonate solution (215g), generating sodium chloroacetate 354.8 g (content 32.8%); be warming up to 50 ℃, then dropwise add 165.0g (1.01mol) of sodium cyanide aqueous solution of mass concentration 30%, when the reaction temperature reaches 85-90 ℃, stop heating and start cooling, when the reaction temperature When the temperature reaches 105°C, the reaction is completed, and cooled to room temperature to obtain an aqueous solution of sodium cyanoacetate;

[0027] (2) Acidification reaction: add mass concentration 30% hydrochloric acid (127.8g, 1.05mol) to the aqueous sodium cyanoacetate solution obtained in step (1) to acidify to obtain 495.1g of a mixture containing cyanoacetic acid and sodium chloride;

[0028] (3) Distilled ...

Embodiment 2

[0032] (1) Cyanide reaction: 96.8g of chloroacetic acid (content 98%, 1.0mol) and 70g of water were stirred and dissolved, and neutralized to pH=6.5-7.0 with 25% aqueous sodium carbonate solution (215g), generating sodium chloroacetate 354.8 g (content 32.8%); be warming up to 50 ℃, then dropwise add 179.7g (1.1mol) of sodium cyanide aqueous solution of mass concentration 30%, when the reaction temperature reaches 85-90 ℃, stop heating and start cooling, when the reaction temperature When the temperature reaches 105°C, the reaction is completed, and cooled to room temperature to obtain an aqueous solution of sodium cyanoacetate;

[0033] (2) Acidification reaction: add mass concentration 33% hydrochloric acid (110.6g, 1.0mol) to the sodium cyanoacetate aqueous solution obtained in step (1) to acidify to obtain 474.9g of a mixture containing cyanoacetic acid and sodium chloride;

[0034](3) Distilled water desalination: turn on vacuum, control the vacuum degree of the system to...

Embodiment 3

[0038] (1) Cyanide reaction: 96.8g of chloroacetic acid (content 98%, 1.0mol) and 70g of water were stirred and dissolved, and neutralized to pH=6.5-7.0 with 25% aqueous sodium carbonate solution (215g), generating sodium chloroacetate 354.8 g (content 32.8%); be warming up to 50 ℃, then dropwise add 171.5g (1.05mol) of sodium cyanide aqueous solution of mass concentration 30%, when the reaction temperature reaches 85-90 ℃, stop heating and start cooling, when the reaction temperature When the temperature reaches 105°C, the reaction is completed, and cooled to room temperature to obtain an aqueous solution of sodium cyanoacetate;

[0039] (2) Acidification reaction: add mass concentration 36% hydrochloric acid (111.5g, 1.1mol) to the sodium cyanoacetate aqueous solution obtained in step (1) to acidify to obtain 439.8g of a mixture containing cyanoacetic acid and sodium chloride;

[0040] (3) Distilled water desalination: turn on the vacuum, control the vacuum degree of the sys...

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 preparation method of cyanoacetic acid and derivatives thereof. Evaporation concentration of part of water in a mixture containing cyanoacetic acid and sodium chloride is carried out, and filtration is performed to remove the precipitated part of sodium chloride solids, thus avoiding the disadvantages of mass decomposition of cyanoacetic acid and low yield caused by the traditional distillation desalination, at the same time after desalination, the solution containing cyanoacetic acid and sodium chloride is separated into a cyanoacetic acid solution and a sodium chloride solution by continuous chromatography, thus avoiding decomposition in a cyanoacetic acid concentration process. The method provided by the invention has the advantages of simple operation, low production cost, high product yield and small amount of three wastes, and is a clean and environment-friendly production method, and can acquire a low chlorine ion content cyanoacetic acid solution or high content solid cyanoacetic acid product and derivatives thereof.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis and separation, and relates to a preparation method of cyanoacetic acid and derivatives thereof. Background technique [0002] Cyanoacetic acid is an important intermediate in the production of medicines, dyes, and pesticides, and is used in the production of malonic acid, cyanoacetate, malonate, α-methyl cyanoacrylate, vitamin B6, caffeine, and cream uran . [0003] The traditional production process uses chloroacetic acid, sodium carbonate, and sodium cyanide as raw materials, and is obtained through neutralization, cyanation, acidification, and dehydration under reduced pressure. However, the content of the solid cyanoacetic acid product obtained by this method is only about 90%, and the water content and salt content are relatively high, which limits its application. Because the concentration of cyanoacetic acid in the cyanoacetic acid mixed solution is low, and the conten...

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): C07C253/14C07C253/30C07C255/19C07C51/08C07C55/08C07C67/08C07C69/38
Inventor 丁永良徐代行张飞刘佳唐大家何咏梅陈依柔
Owner CHONGQING UNISPLENDOUR CHEM
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com