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Preparation method of dicyclohexylcarbodiimide

A technology of dicyclohexylcarbodiimide and dicyclohexylurea, which is applied in the field of preparation of dicyclohexylcarbodiimide, can solve the problems of unstable industrial production, large potential safety hazards, etc., and achieves improved stability and product yield. efficiency, easy operation and simple process

Inactive Publication Date: 2019-01-18
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can optimize the yield and purity of carbodiimide, but it is easy to decompose to produce highly toxic phosgene, which has great safety hazards and is not stable enough for industrial production

Method used

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  • Preparation method of dicyclohexylcarbodiimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 50g of DCU, 300mL of dichloromethane, and 0.1g of pyridine into a dry 500mL three-necked flask, stir evenly, dissolve 37.8g of chloroacetyl chloride in 100mL of dichloromethane and add it dropwise to the three-necked flask, and control the dropping time to 3h. The dropwise addition temperature is 5-10°C. After the dropwise addition, raise the temperature to 60°C and keep stirring for 5 hours. After the reaction, pass through ammonia gas to adjust the pH to neutral, and then filter with suction. Distilled under reduced pressure at a pressure of 1.54KPa, collected fractions at 153-156°C, and vacuum-dried to obtain the product with a purity of 97.1% and a yield of 92.8%.

Embodiment 2

[0024] Put 50g of DCU, 300mL of acetonitrile, and 0.15g of pyrrole into a dry 500mL three-necked flask, stir evenly, dissolve 37.8g of chloroacetyl chloride in 100mL of acetonitrile, and drop them into the three-necked flask. The dropping time is controlled to be 3 hours, and the dropping temperature is 5-10°C, after the dropwise addition, raise the temperature to 60°C and keep stirring for 5 hours. After the reaction, pass through ammonia gas to adjust the pH to neutral, and then filter with suction. Distill under reduced pressure, collect fractions at 153-156°C, and vacuum dry to obtain the product with a purity of 92.7% and a yield of 85.4%.

Embodiment 3

[0026] Put 50g of DCU, 300mL of acetone, and 0.15g of pyridine into a dry 500mL three-necked flask, stir evenly, dissolve 37.8g of chloroacetyl chloride in 100mL of acetone, and drop them into the three-necked flask. The dropping time is controlled to be 3 hours, and the dropping temperature is 5-10°C, after the dropwise addition, raise the temperature to 60°C and keep stirring for 5 hours. After the reaction, pass through ammonia gas to adjust the pH to neutral, and then filter with suction. Distill under reduced pressure, collect fractions at 153-156°C, and vacuum dry to obtain the product with a purity of 93.2% and a yield of 90.9%.

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Abstract

The invention belongs to the technical field of fine chemical engineering and in particular relates to a preparation method of dicyclohexylcarbodiimide. The preparation method comprises the followingsteps: dissolving chloroacetyl chloride in a solvent to obtain a solution A; stirring dicyclohexylurea, a catalyst and a solvent uniformly to obtain a solution B; dropwise adding the solution A into the solution B at a certain temperature; then carrying out an insulating reaction; after the reaction, adding a pH regulator to regulate the solution to be neutral; carrying out suction filtration on the reaction solution; distilling the filtrate at constant pressure to remove the solvent; and then carrying out distillation at a reduced pressure to obtain dicyclohexylcarbodiimide. The preparation method of dicyclohexylcarbodiimide is simple in process, the reaction stability and the product yield are improved greatly, dicyclohexylcarbodiimide can be produced industrially on a large scale, and the preparation method has the advantages of being simple and feasible and simple to operate.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of dicyclohexylcarbodiimide. Background technique [0002] Dicyclohexylcarbodiimide (DCC) is a white or light yellow crystal with a very low melting point. It is widely used in organic, pharmaceutical, dye and biosynthesis fields. It is often used as a dehydrating agent for aldehydes, ketones, esters, and amino acids. Synthesis of other compounds. [0003] At present, the methods for synthesizing dicyclohexylcarbodiimide mainly contain the following methods: thiourea method, urea method and phosgene method. The patent of CN101096349A has reported a kind of technology that adopts thiourea method to produce dicyclohexyl carbodiimide, and it adopts cyclohexane and carbon disulfide to react to generate dicyclohexyl thiourea and sodium sulfide, and dicyclohexyl thiourea passes through sodium hypochlorite secondary Oxidative dehydrogenation to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
CPCC07C267/00C07C2601/14
Inventor 王冠庆梁寒冰崔宝龙李凯
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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