Catalyst for reactive synthesis of carbamate by urea and organic carbonic ester as well as preparation method and application thereof

A carbamate and catalyst technology, which is applied in the preparation of organic compounds, carbamic acid derivatives, organic chemistry, etc., can solve the problems of difficult recycling, difficult promotion of lead catalyst toxicity, high price, etc., and achieve easy recycling Reuse, easy availability, no polluting effect

Inactive Publication Date: 2012-04-04
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These catalysts are homogeneous catalysts, which are not only expensive, but also difficult to recycle
Afterwards, Li Huiquan and others used lead methoxide for this reaction to prepare phenylcarbamate (Petrochemical Industry, 2009, 38(2): 145-148), but the toxicity of lead catalysts made it difficult to popularize

Method used

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  • Catalyst for reactive synthesis of carbamate by urea and organic carbonic ester as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Accurately weigh 10.0gZrO 2 and 0.6gLi 2 CO 3 , will Li 2 CO 3 Dissolved in 6.0 g of deionized water and then impregnated into ZrO 2 After drying at room temperature for 4 h, place it in an oven and dry at 110 °C for 12 h, then transfer to a muffle furnace and bake at 450 °C for 6 h in an air atmosphere to produce Li 2 O / ZrO 2 catalyst.

[0031] 30.0g dimethyl carbonate, 3.18g 1,3-diphenylurea and 0.5g Li 2 O / ZrO 2 Catalyst is placed in 100mL autoclave, passes N 2 After replacing the air in the autoclave, the autoclave was sealed, and the temperature was raised to 160° C. under stirring conditions, and kept for 4 hours. Afterwards, the reaction was stopped, and the reaction product was taken out after cooling down to room temperature, and subjected to chromatographic analysis. The conversion rate of 1,3-diphenylurea was 91.3%, and the yield of phenylcarbamate was 74.3%.

Embodiment 2

[0033] Accurately weigh 10.0gCeO 2and 0.5gLiNO 3 , the LiNO 3 Dissolved in 5.0 g of deionized water and impregnated into CeO 2 After drying at room temperature for 4 hours, place it in an oven to dry at 110°C for 12 hours, then transfer it to a muffle furnace and bake it at 450°C for 4 hours in an air atmosphere to produce Li 2 O / CeO 2 catalyst.

[0034] 30.0g of dimethyl carbonate, 3.18g of 1,3-diphenylurea and 0.5g of the above Li 2 O / CeO 2 The catalyst was placed in a 100mL autoclave, and under the same reaction conditions as in Example 1, the conversion rate of 1,3-diphenylurea was 92.4%, and the yield of phenylcarbamate was 85.8%.

Embodiment 3

[0036] 30.0g dimethyl carbonate, 2.12g1,3-diphenylurea and 0.5g Li 2 O / CeO 2 The catalyst was placed in a 100mL autoclave, and under the same reaction conditions as in Example 1, the conversion rate of 1,3-diphenylurea was 94.5%, and the yield of phenylcarbamate was 87.2%.

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Abstract

The invention discloses a catalyst for reactive synthesis of carbamate by urea and organic carbonic ester, which comprises the following components in percentage by weight: 1-20wt% of alkali metal oxide and the balance of carrier, wherein the alkali metal is selected from more than two of Li, Na, K, Rb and Cs; and the carrier is an oxide carrier or a molecular sieve carrier. The catalyst has the advantages of simple preparation process, low raw material cost, high target product yield and no pollution on the environment.

Description

technical field [0001] The invention belongs to a preparation method and application of a catalyst for synthesizing carbamate, in particular to a catalyst suitable for preparing carbamate compounds by reacting ureas and organic carbonates, and a preparation method and application thereof. Background of the invention [0002] Methyl carbamate is an important class of fine chemicals with a wide range of uses, such as pesticides, medicines, synthetic resin modification, intermediates in organic synthesis, and protection of amino groups in organic synthesis. Carbamate compounds have been used as sedative drugs in medicine for a long time, and phenyl-substituted ethyl or propylene glycol dicarbamate has also been used as anti-inflammatory agents, muscle relaxants, analgesics, anti-epileptic drugs, etc. Very good curative effect. Carbamate compounds are used as insecticides, acaricides, herbicides and fungicides in pesticides, and have formed a large category of pesticides with m...

Claims

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Application Information

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IPC IPC(8): B01J23/04B01J23/10B01J29/08C07C269/00C07C271/28C07C271/12C07C271/58
Inventor 王军威亢茂青王心葵冯月兰李其峰赵雨花殷宁张清运
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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