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Production of carbaminate by amine reacted with dimethyl ester carbonate

A technology of dimethyl carbonate and carbamate, which is applied in the field of amine and dimethyl carbonate reaction to make carbamate, which can solve the problems of easy deactivation of the catalyst and achieve the effects of high purity, simple separation and simple system

Inactive Publication Date: 2003-06-18
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, the synthesis process also involves the use of high temperature, high pressure and toxic carbon monoxide, and the catalyst is easily deactivated, which limits its application and promotion.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0015] In a 1000 ml high-pressure reactor, 20 grams of n-hexylamine and 20 grams of 1-methyl-3-butylimidazolium chloride ionic liquid were added, and the temperature was raised to 170° C. under stirring. After reacting for 1 hour, it was cooled to room temperature, and then 100 ml of distilled water was added to the reaction mixture to precipitate n-hexyl carbamate crystals with a purity of 99% and a yield of 98%. The 1-methyl-3-butylimidazolium chloride ionic liquid was reused 3 times (Example 2-4).

[0016] Table 1 Reaction of n-hexylamine and dimethyl carbonate to prepare n-hexyl carbamate Reuse cycle times 1 2 3 4 n-hexylamine conversion rate% 100 100 100 100 n-hexyl carbamate yield% 99 99 98 99 n-hexylamino Formate purity % 99 99 99 99

Embodiment 5

[0018] In a 1000 ml high-pressure reactor, 20 grams of cyclohexylamine and 20 grams of 1-butyl-3-methylimidazolium chloride ionic liquid were added, and the temperature was raised to 170° C. under stirring. After reacting for 1 hour, it was cooled to room temperature, and then 100 ml of distilled water was added to the reaction mixture to precipitate cyclohexyl carbamate crystals. The purity of the product was greater than 86%, and the yield was 85%. Example 6.

Embodiment 6

[0019] In a 1000 ml high-pressure reactor, 20 grams of cyclohexylamine and 20 grams of 1-methyl-3-butyl-imidazolium fluoroborate ionic liquid were added, and the temperature was raised to 170° C. under stirring. After reacting for 1 hour, it was cooled to room temperature, and then 100 ml of distilled water was added to the reaction mixture to precipitate cyclohexyl carbamate crystals. The purity of the product was greater than 89%, and the yield was 85%.

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Abstract

A process for preparing aminoformate from amine and dimethyl carbonate (DMC) features that under the existance of ionic liquid as solvent and catalyst system, the amine and DMC take part in catalytic oxo reaction at 40-200 deg.C for 0.5-5 hr. Its advantages are high output rate (more than 98%), high purity (more than 98%), high reaction activity, and easy recovery and cyclic use of catalyst.

Description

technical field [0001] The invention relates to a method for preparing carbamate by reacting amine and dimethyl carbonate. Background technique [0002] As a class of important organic reaction intermediates, isocyanates are widely used in industry, agriculture, medicine and health. These compounds are widely used in the synthesis of polyisocyanates, polyurethanes, polyureas, polymer adhesives, insecticides, herbicides, etc. At the same time, the demand for various isocyanates continues to grow with the development of society. At present, isocyanates are mainly prepared by reacting corresponding amine compounds with phosgene. Phosgene is a highly toxic compound, and a large amount of highly corrosive hydrogen chloride is generated during the reaction. Therefore, it often leads to equipment corrosion, phosgene leakage, environmental pollution and personal injury. [0003] With the increasing environmental pollution around the world, governments of various countries are co...

Claims

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Application Information

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IPC IPC(8): C07C269/04C07C271/08
CPCY02P20/54
Inventor 邓友全石峰顾彦龙唐爱华彭家建
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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