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Method for synthesizing cyclohexyl carbamate

A technology of cyclohexyl carbamate and dicyclohexyl urea, which is applied in the field of synthesizing cyclohexyl carbamate, can solve the problems of reducing the effective utilization rate of functional groups of reaction raw materials, limiting research progress and industrialization process, and poor atom economy. Achieve the effects of strong practicability, high reaction selectivity and yield, and easy separation

Active Publication Date: 2010-06-30
青岛奥立科新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first two reactions use CO as the carbonyl source, noble metal compounds as catalysts, and are carried out under high temperature and pressure, and the reaction conditions are harsh, which limits their research progress and industrialization process.
For the latter two reactions, although the reaction conditions are mild and the operation process is simple, they produce alcohols and amines by-products respectively, which reduces the effective utilization of the functional groups of the reaction raw materials, and the atom economy is poor.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 2 liter autoclave, add 1300 grams of dimethyl carbonate (DMC), 270 grams of N, N'-dicyclohexyl urea (DCU), catalyst ZnO / SiO 2 25 grams, at a temperature of 150° C., a pressure of 1.5 MPa and a rotation speed of 500 rpm, the temperature, pressure and rotation speed were maintained for 6 hours and the reaction was completed. When the temperature is cooled down to room temperature, open the reaction kettle to take a sample to obtain a clear liquid and a sample with a catalyst at the bottom, and take the clear sample for direct gas chromatography analysis. In addition, the sample is filtered, the catalyst is separated, dried and used next time. The filtrate was distilled at 80° C. and 60 mmHg, the DMC was recovered and could be recycled, and a white solid was obtained at the same time. Then raise the temperature to 140°C, keep the vacuum constant, and distill to obtain methyl cyclohexylcarbamate. The residue is a small amount of by-products and unreacted DCU, and the...

Embodiment 2

[0034] In a 2-liter autoclave, add 1300 grams of dimethyl carbonate (DMC), 200 grams of N, N'-diphenylurea (DPU), catalyst ZnO / SiO 2 15 grams, at a temperature of 150° C., a pressure of 1.5 MPa and a rotating speed of 500 rpm, the temperature, pressure and rotating speed were maintained for 6 hours and the reaction was completed. When the temperature is cooled down to room temperature, the reactor is opened to take a sample to obtain a clear liquid and a sample with a catalyst at the bottom, and the clear sample is directly subjected to liquid chromatography analysis. In addition, the sample is filtered, the catalyst is separated, dried and used next time. The filtrate was distilled at 80° C. and 60 mmHg, the DMC was recovered and could be recycled, and a white solid was obtained at the same time. Then raise the temperature to 150°C, keep the vacuum degree constant, distill to obtain methyl cyclohexylcarbamate, and the residue is a small amount of by-products. Chromatographi...

Embodiment 3

[0036] In a 2 liter autoclave, add 1500 grams of diethyl carbonate (DEC), 200 grams of N, N'-dicyclohexylurea (DCU), catalyst CeO 2 / ZrO 215 grams, at a temperature of 150° C., a pressure of 1.5 MPa and a rotating speed of 500 rpm, the temperature, pressure and rotating speed were maintained for 6 hours and the reaction was completed. When the temperature is cooled down to room temperature, open the reactor to take a sample to obtain a clear liquid and a sample with a catalyst at the bottom, and the clear sample is directly subjected to chromatographic analysis. In addition, the sample is filtered, the catalyst is separated, dried and used next time. The filtrate was distilled at 100°C and 60mmHg, the DEC was recovered and could be recycled, and a white solid was obtained at the same time. Then raise the temperature to 150°C, keep the vacuum degree constant, distill to obtain ethyl cyclohexyl carbamate, and the residue is a small amount of by-products. The chromatographic a...

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Abstract

The invention discloses a method for synthesizing cyclohexyl carbamate. The invention chooses a supported metal oxide solid catalyst to catalyze dialkyl carbonate and N,N'-dicyclohexylurea to obtain the product. The method is mainly characterized in that reaction condition is relatively mild; the catalyst is easy to recycle and good in repeated use; the reaction is atom economy; and the separatedproduct has high purity.

Description

technical field [0001] The present invention relates to a kind of method of synthesizing cyclohexyl carbamate, specifically, the present invention is a kind of method of catalyzing dialkyl carbonate and N, N'-dicyclohexyl urea synthetic cyclohexyl carbamate. Background technique [0002] As an important organic reaction intermediate, isocyanate is the main raw material for polyurethane synthesis. It can be widely used in polymer materials such as polyurethane, coatings, fuels and pesticides. It has a very wide range of uses in industry, agriculture, medicine and health. . [0003] my country's polyurethane industry started relatively late, but since the 1990s, with the sustained and rapid development of the national economy, the demand for isocyanate and polyurethane in related industries has increased at an annual growth rate of 12% and 10%, respectively, while domestic production capacity Seriously inadequate. In the traditional isocyanate synthesis industry, it is mainly...

Claims

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Application Information

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IPC IPC(8): C07C271/24C07C269/02
CPCY02P20/584
Inventor 邓友全郭晓光尚建鹏石峰李健马祥元崔新江张宏哲何昱德
Owner 青岛奥立科新材料科技有限公司
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