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

Production method for preparing N,N'-dicyclohexylcarbodiimide (DCC) by recycling wastewater

A technology of dicyclohexylcarbodiimide and a production method, which is applied in the field of organic compound synthesis, can solve the problems of high cost, increased cost, environmental pollution by salty sewage, and achieves the effects of reducing discharge and reducing impact

Inactive Publication Date: 2015-01-07
山东巨业精细化工有限公司
View PDF5 Cites 10 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] DCU can be treated with phosphorus pentoxide (P 2 o 5 ) dehydration in pyridine or react with benzenesulfonyl chloride to generate DCC, the method yield is low and the cost is high
DCU can also react with phosgene first, and then react with amine to generate DCC. This method uses toxic phosgene, which is not conducive to the operating environment
[0007] Japanese patent JP 8-231491A discloses a production process in which DCU is used as a raw material to be oxidized by phosphorus oxychloride and then neutralized with lye to reduce it to DCC. This production process will produce a large amount of salty sewage , the discharge of a large amount of saline sewage will pollute the environment, and the treatment of this large amount of saline sewage to meet the discharge requirements will greatly increase the cost
Chinese patent CN101928237A discloses a production process for preparing DCC by regenerating DCU produced after use of DCC. This process still has the problem of treating a large amount of salty sewage

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
  • Production method for preparing N,N'-dicyclohexylcarbodiimide (DCC) by recycling wastewater
  • Production method for preparing N,N'-dicyclohexylcarbodiimide (DCC) by recycling wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Put 5kg of N,N'-dicyclohexyl urea raw material into 10kg of water, stir and soak for 40min, centrifuge the soaked DCU for dehydration, and then dry it in an oven at 110--120℃ until the water content is lower than 0.5%.

[0040] 175 g of chloroform was added into the three-necked flask, and 40.0 g of dried DCU was added under stirring. Weigh 30g of phosphorus oxychloride and add it to a 250mL dropping funnel. Phosphorus oxychloride was added dropwise to the three-necked flask under stirring, and the addition was completed within 30 minutes. After the addition was complete, the reaction was maintained at 55-60°C for 2 hours. Pour the reaction solution into the dropping funnel.

[0041] Add 400 g of waste water to the three-necked flask, add 45 g of solid sodium hydroxide under stirring, and stir for 20 minutes until all the sodium hydroxide is dissolved. Then the reaction solution was added dropwise to the three-neck flask, and the addition was completed in 60 minutes....

Embodiment 2

[0045] Referring to Example 1, the difference is that dichloromethane is used instead of chloroform. The reaction temperature after the dropwise addition of phosphorus oxychloride is 40-42°C; the neutralization reaction temperature is controlled below 40°C. The yield of DCC was 81.5%, and the purity was 99.4%.

[0046] It can be seen that in the present invention, the waste water containing inorganic salt produced by the reaction is separated from the system by filtration and then reused as a raw material, which reduces the discharge of waste water and the impact on the environment. At the same time, the use of the waste water containing saturated phosphate and sodium chloride of the present invention has no obvious influence on the product yield and purity of the DCC process prepared by DCU.

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 for preparing N,N'-dicyclohexylcarbodiimide (DCC) by recycling wastewater, belonging to the technical field of organic compound synthesis. The method solves the problem of unmanageable brine sewage at present. The method comprises the following steps: washing N,N'-dicyclohexylurea (DCU) generated after using DCC with water to remove impurities, reacting with an oxidizer in an organic solvent, dropwisely adding the reaction solution into an alkali water solution to carry out neutralization reaction, filtering the neutralization reaction product, standing to stratify, and carrying out distillation separation on the organic layer to obtain the DCC product, wherein the distilled solvent is directly recovered; and filtering out inorganic salts from the water layer to obtain recovered water for preparing the alkali solution. The DCU generated after using the DCC is recovered to obtain the DCC; and the generated brine wastewater is recycled, thereby reducing the discharge of the brine sewage and greatly lowering the brine sewage treatment.

Description

technical field [0001] The invention relates to a production method of N,N'-dicyclohexylcarbodiimide, in particular to an environmentally friendly production method for the regeneration of N,N'-dicyclohexylcarbodiimide, which belongs to the synthesis of organic compounds technology field. Background technique [0002] N,N'-Dicyclohexylcarbodiimide (DCC for short) is a shrinking agent commonly used in organic synthesis and pharmaceutical manufacturing industries. It can dehydrate two molecules that cannot react originally to form a chemical bond. In my country, it is mainly used for the synthesis of products such as amikacin and glutathione. [0003] The structural formula of N,N'-dicyclohexylcarbodiimide is: [0004] [0005] DCC is used as a shrinking agent, and its reaction product is N,N'-dicyclohexyl urea (DCU). DCU is toxic and its discharge will pollute the environment. Utilizing the regeneration of DCU to prepare DCC can realize the regeneration and utilization...

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): C07C267/00
Inventor 高鑫王国德高健李雪梅
Owner 山东巨业精细化工有限公司
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