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Supported ionic liquid catalyst and preparation and applications thereof

A technology of ionic liquid and catalyst, which is applied in the preparation and application of green reaction medium, can solve the problems of difficult separation and recovery of catalyst, low product yield, etc., and achieve the effect of overcoming low catalyst activity and high catalytic activity

Inactive Publication Date: 2011-05-04
HEBEI UNIV OF TECH
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  • Abstract
  • Description
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Problems solved by technology

[0005] The invention solves the problems of low product yield and difficult catalyst separation and recovery in the prior art, thereby providing a supported ionic liquid catalyst for synthesizing methyl phenylcarbamate by aniline carbonyl methoxylation and its preparation method

Method used

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preparation example Construction

[0015] The document of the preparation method of ionic liquid used in the present invention:

[0016] 1-Ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole Tetrafluoroborate, 1-ethyl-3-methylimidazolium hexafluorophosphate and 1-butyl-3-methylimidazolium hexafluorophosphate; according to Zhang Yang (Beijing University of Aeronautics and Astronautics, 2002 , dissertation) to synthesize 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole acetate, ethylpyridine acetate, butylpyridine acetate four ionic liquids such as salt; 1-butyl-3-methylimidazole bromide and 1-ethyl-3-methylimidazole bromide are referenced by Song Shaoqing (Chemical Technology and Development, 2006, 35(6): 8~ 10) Synthesis of the route provided; trihexyltetradecylphosphine bromide was directly purchased from Bailingwei Chemical Technology Co., Ltd. The specific embodiment of the preparation of supported ionic liquid and its application in the synthetic reaction of methyl phenylcarba...

Embodiment 1

[0018] Take by weighing anhydrous zinc acetate 1.821g, ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate ([emim]BF 4 ) 18.21 g were put into a three-necked flask in sequence, and stirred at 150° C. for 5 h to obtain supported anhydrous zinc acetate ionic liquid (the mass ratio of anhydrous zinc acetate to ionic liquid was 0.1).

[0019] Measure aniline (AN) 6mL, dimethyl carbonate (DMC) 39mL (V DMC :V AN =6.5, the sum of the two masses is 47.85g), the support anhydrous zinc acetate ionic liquid 7.286g (anhydrous zinc acetate accounts for 1.4% of the sum of AN and DMC quality) of above-mentioned preparation is put into successively with magnetic stirring In a 100mL autoclave, replace the air in the autoclave with nitrogen and start to heat up. After reaching the set temperature of 160°C, start timing (the pressure is not the specific control condition of this reaction. After heating to a certain temperature, the system will automatically generate a certain pressure. T...

Embodiment 2

[0021] Weigh 1.821g of anhydrous zinc acetate and 6.07g of ionic liquid 1-ethyl-3-methylimidazole bromide ([emim]Br) into a three-necked flask in turn, and stir at 0°C for 10h to obtain a supported anhydrous Zinc acetate ionic liquid (mass ratio of anhydrous zinc acetate to ionic liquid: 0.3).

[0022] Measure aniline 6mL and dimethyl carbonate 39mL respectively (V DMC :V AN =6.5, the sum of the two masses is 47.85g), the support anhydrous zinc acetate ionic liquid 7.286g (anhydrous zinc acetate accounts for 3.5% of the sum of AN and DMC quality) of above-mentioned preparation is put into successively with magnetic stirring In a 100mL autoclave, replace the air in the autoclave with nitrogen and start to heat up. After reaching the set temperature of 70°C, start timing. After reacting for 7 hours, stop heating. After cooling to room temperature, take the reaction solution for liquid phase analysis to obtain benzene The yield of methyl carbamate was 87.9%, and the selectivity...

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Abstract

The invention belongs to the preparation of green reaction media and application, and relates to a supported ionic liquid catalyst and preparation and applications thereof. The catalyst consists of anhydrous zinc acetate and ionic liquid with the mass ratio of 0.1-1:1. The supported ionic liquid catalyst is applied in the carbonilino methoxylation reaction of and easy to be prepared; and the catalytic activity is high, the highest yield of N-phenyl carbamate can reach 98.9 percent, the reaction product can be separated from reaction liquid after simple distillation and extraction, and the recycled ionic liquid can be recycled.

Description

technical field [0001] The invention belongs to the preparation and application of a green reaction medium, in particular to a supported ionic liquid catalyst and its preparation method and application. Background technique [0002] Methyl phenylcarbamate is an important intermediate for the non-phosgene synthesis of diphenylmethane diisocyanate (MDI). The synthesis methods include oxidative carbonylation of aniline, reductive carbonylation of nitrobenzene, alcoholysis of phenylurea and alcoholysis of urea. The catalysts used in the oxidative carbonylation of aniline or the reductive carbonylation of nitrobenzene are mainly noble metals (such as Ru, Rh, Pd, etc.) or their complexes, which makes the production cost of the process higher; the alcohol of phenylurea The solution method mainly uses lead compounds as catalysts, which is not friendly to the environment, and the cost of the raw material phenylurea is relatively high; the reaction system of the urea alcoholysis meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C271/28B01J31/04B01J31/02B01J37/04C07C269/04
Inventor 赵新强王娜安华良王延吉
Owner HEBEI UNIV OF TECH
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