A kind of production method of recycling waste water to prepare n,n'-dicyclohexylcarbodiimide

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, unfavorable operating environment, etc., and achieves the effects of reducing emissions and reducing impact

Inactive Publication Date: 2016-06-29
山东巨业精细化工有限公司
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  • 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

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  • A kind of production method of recycling waste water to prepare n,n'-dicyclohexylcarbodiimide
  • A kind of production method of recycling waste water to prepare n,n'-dicyclohexylcarbodiimide

Examples

Experimental program
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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.

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Abstract

The invention discloses a production method for preparing N,N'-dicyclohexylcarbodiimide by recycling waste water, and belongs to the technical field of organic compound synthesis. It solves the problem that the existing salty sewage is difficult to treat. The N,N'-dicyclohexylurea produced after the use of N,N'-dicyclohexylcarbodiimide is washed with water to remove impurities, and then reacted with an oxidant in an organic solvent, and the reaction solution is added dropwise to an aqueous alkali solution for Neutralization reaction, the neutralization reaction product is filtered and then stratified, the organic layer is distilled and separated to obtain the DCC product, and the evaporated solvent is directly reused; the water layer is filtered to remove the inorganic salt and reused as the water required for the preparation of the lye. The production method reuses the DCU produced after the use of DCC to obtain DCC, and at the same time, recycles the generated saline wastewater, which reduces the discharge of saline wastewater and greatly reduces the treatment of saline wastewater.

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

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Application Information

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Patent Type & Authority Patents(China)
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
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