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Carbazic acid alcohol ester synthesis method

An alcohol formate and hydrazine-based technology, which is applied in the fields of CO2 capture and chemical utilization, can solve the problems of difficulty in wide application and high cost, and achieve the effects of reducing production costs, easy temperature control, and realizing CO2 emission reduction.

Inactive Publication Date: 2014-08-13
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high cost of this technology, it is difficult to be widely used, and in case of geological disasters and other events, the stored CO 2 will be released again

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1, the gas-liquid reactor used is a bubbling reactor with a volume of 1L, and 1molL is added thereto -1 Add 0.5 L of hydrazine hydrate, then add 0.5 mol of benzyl alcohol, the ratio of the amount of hydrazine hydrate to benzyl alcohol is 1:1, then add sodium sulfate as a catalyst, and make the concentration of the catalyst 0.1 molL -1 , adjust the pH value of the solution to 5 with hydrochloric acid, and then pass through CO 2 gas (i.e. CO 2 Concentration is 100%), control CO 2 The flow rate makes the CO 2 The gas-liquid contact time between gas and hydrazine hydrate solution and alcohol is 0.1 second, and the reaction temperature is 80°C. Benzyl carbazate is generated in the bubbling reactor and separated from the water phase. After about five minutes, the hydrazine hydrate reacts completely. The mixture was transferred to a separatory funnel and extracted with ethyl acetate, dried over anhydrous magnesium sulfate and then subjected to vacuum distillation to...

Embodiment 2

[0016] Embodiment 2: The gas-liquid reactor used is a bubbling reactor with a volume of 1L, and 2molL is added thereto -1 Add 0.5 L of hydrazine hydrate, then add 2 mol of benzyl alcohol, the ratio of the amount of hydrazine hydrate to benzyl alcohol is 1:2, then add 4-lutidine as a catalyst, so that the concentration of the catalyst is 0.001 molL -1 , adjust the pH value of the solution to 11 with sodium hydroxide, and then pass through CO 2 Mixed gas with air, CO 2 Volume percentage concentration is 20%, control CO 2 The flow rate makes the CO 2 The gas-liquid contact time between gas and hydrazine hydrate solution and alcohol is 1 second, and the reaction temperature is 40°C. Benzyl carbazate is generated in the bubble reactor, and it is separated from the water phase. After about half an hour, the hydrazine hydrate reacts completely. The mixture was transferred to a separatory funnel and extracted with ethyl acetate, dried over anhydrous magnesium sulfate and then subje...

Embodiment 3

[0017] Embodiment 3: The gas-liquid reactor used is a bubbling reactor with a volume of 1L, and 6molL is added thereto -1 Hydrazine hydrate 0.5L, then add methanol 4.5mol, the ratio of the amount of hydrazine hydrate to benzyl alcohol is 1:1.5, then add N,N'-dicyclohexylcarbodiimide as a catalyst, so that the concentration of the catalyst is 0.01 moL -1 , adjust the pH value of the solution to 10 with sodium hydroxide, and then pass through CO 2 Mixed gas with air, CO 2 Volume percentage concentration is 50%, control CO 2 The flow rate makes the CO 2 The gas-liquid contact time between the gas and the hydrazine hydrate solution and alcohol is 2 seconds, and the reaction temperature is 20°C. In the bubble reactor, methyl carbazate is formed and separated with the water phase. After about 50 minutes, the hydrazine hydrate reacts completely , the mixture was transferred to a separatory funnel and extracted with ethyl acetate, dried over anhydrous magnesium sulfate, and subjec...

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PUM

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Abstract

The present invention discloses a carbazic acid alcohol ester synthesis method, which comprises: adding a hydrazine hydrate solution to a gas-liquid reactor, adding an alcohol, adding a catalyst, and adjusting the pH value to 5-11, wherein the alcohol is one selected from C1-C6 fatty alcohols or is benzyl alcohol, and the catalyst is selected from sodium sulfate, 4-dimethyl pyridine or N,N'-dicyclohexyl carbodiimide; introducing CO2 gas to the gas-liquid reactor, wherein the gas-liquid contact time is 0.1-5 seconds, and the reaction temperature is 20-80 DEG C; and after the hydrazine hydrate in the gas-liquid reactor completely reacts, taking out the reaction product, and purifying to obtain the carbazic acid alcohol ester. According to the method, the flowing CO2 gas is adopted as the raw material, the reaction time is short, the yield is high, the process equipment is simple, and the operation is easy. With the method, the CO2 in the flue gas can be absorbed, the high added value chemical industry product can be produced, the economic value can be created, and CO2 emission reduction and environment protection can be achieved.

Description

technical field [0001] The invention belongs to CO 2 The field of capture and chemical utilization, specifically related to the use of CO 2 Gas synthesis method of carbazate. Background technique [0002] Alcohol carbazate is an important organic intermediate, such as benzyl carbazate, methyl carbazate and ethyl carbazate, etc. The following uses benzyl carbazate as an example to illustrate. Benzyl carbazate is used in the preparation of plant protection agents and transaminase inhibitors, and is widely used in the synthesis of pesticides and medicines. About the synthetic method of benzyl carbazate, existing many documents relate to. For example, the Japanese patent JP9208553 published on August 12, 1997 uses methyl carbazate and benzyl alcohol as raw materials to synthesize benzyl carbazate under the catalysis of sodium methoxide. The disadvantage is that the purity of methyl carbazate is high. The cost is high; U.S. Patent No. 5,756,824 published on May 26, 1998 uses ...

Claims

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Application Information

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IPC IPC(8): C07C281/02
Inventor 赵毅刘威
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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