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Novel solid polymer catalyst for synthesizing dicyclohexylcarbodiimide

A dicyclohexylcarbodiimide, solid polymer technology, applied in the field of new solid polymer catalysts for the synthesis of dicyclohexylcarbodiimide, can solve the problems of harsh conditions, numerous steps, flammability hazards, etc., to achieve the reaction The effect of mild conditions, easy realization, simple synthesis process and high catalytic efficiency

Inactive Publication Date: 2009-09-09
重庆市化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The synthesis process of the solid polymer catalyst disclosed in US 4348337 is complex, with many steps and harsh conditions, the product is not easy to obtain, and the substances used in the preparation process are toxic and flammable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 1) Preparation of catalyst intermediate 1-chloro-3-methyl-3-phosphole-1-oxide

[0013] 137g (1mol) PCl 3 Put it into a three-necked bottle, add 64g (1.1mol) propylene oxide dropwise at 25°C and react for 1 hour, then add 70g of isoprene dropwise to the intermediate, react at 25°C for 1-2 hours, then heat to 100°C , The generated 1,2-dichloropropane was distilled off under reduced pressure to obtain 150 g of 1-chloro-3-methyl-3-phosphole-1-oxide.

[0014] 2) Preparation of monomer (diallyl ether-1-diethanolamino-3-methyl-3-phosphole-1-oxide)

[0015] Add 53.0g diethanolamine and 55.0g triethylamine to 75.0g (0.5mol) 1-chloro-3-methyl-3-phosphole-1-oxide to react at normal temperature, filter to remove salt, add certain Amount of liquid caustic soda is added dropwise to 85.0g chloropropene. The temperature of the whole reaction was below 50°C, and the reaction was completed dropwise for 1 hour, the brine was filtered, and impurities were distilled off under reduced pre...

Embodiment 2

[0018] Embodiment 2: Phosphorous heterocycle solid-phase polymer catalyst is used for synthesizing DCC

[0019] Operation steps: Add a certain amount of cyclohexyl isocyanate and solvent into a 500ml three-neck bottle, then add a phosphorus heterocyclic solid-phase catalyst, and when the temperature is slowly raised to a certain temperature, tail gas will be generated (tail gas is absorbed by dilute NaOH solution), and the reflux reaction will continue for 8 hours At this time, there is basically no exhaust gas overflow, stop heating and cool down. The reaction liquid is filtered, and the filter cake is used as a catalyst, which can be recycled and reused. The filtrate is distilled off the n-hexane solvent in the distillation device under reduced pressure, and the fraction at 130-135°C / 4-5mmHg is collected to obtain the product dicyclohexylcarbodiimide. The product is a white solid, which is recrystallized and centrifuged to obtain 99.0% DCC.

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PUM

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Abstract

The invention discloses a preparation method for a solid organophosphorus catalyst for synthesizing dicyclohexylcarbodiimide and use. The preparation process for the solid polymer catalyst is characterized in that an intermediate obtained by reaction of PCl3 and propylene oxide is orderly reacted with isoprene, diethanolameine, alkali and allyl chloride to generate monomers of diallyl ether-1-diethanolamine-3-methyl-3-phosphol-1-oxides which are initiated by BPO to generate the solid organophosphorus polymer catalyst. The catalyst is used for catalyzing and condensing cyclohexyl isocyanate to obtain the dicyclohexylcarbodiimide, the dosage is between 0.1 and 0.5 percent, and the reaction temperature for removing carbon dioxide by condensation is between 50 and 170 DEG C. The catalyst has simple synthesis process and low cost and can be recycled.

Description

technical field [0001] The invention relates to a preparation method and use of an organophosphorus solid-phase catalyst for synthesizing dicyclohexylcarbodiimide. Background technique [0002] With the development of peptide and protein chemistry, people have designed and synthesized various types of condensing agents to meet the requirements of peptide and protein synthesis. The condensing agent dicyclohexylcarbodiimide (Dicyclohexylcarbodiimide, DCC) proposed by Sheehan and Hess in 1955 is representative. It is widely used in medicine, health products, cosmetics, biological agents and other organic synthesis fields. Therefore, the catalysts used for the synthesis of DCC have become a research hotspot. In the 1960s to 1980s, organophosphorus catalysts, which appeared continuously in the 1960s and 1980s, became mainstream through the condensation of isocyanates to carbodiimides. They were not only used to synthesize carbodiimides from monoisocyanates and polycarbodiimides...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C251/02C07C249/02C08F130/02
Inventor 颜邦民吴渝赵丽颖蒋惠李昌杰
Owner 重庆市化工研究院有限公司
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