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The method for the synthesis of methyl benzoate by two still combined phase transfer catalysis

A technology of methyl benzoate and phase transfer catalysis, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of complex post-processing, high production cost, large amount of catalyst, etc., and achieve equipment High cost, achieve recycling and reuse, and reduce emissions

Inactive Publication Date: 2019-07-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] This reaction uses excessive sodium benzoate to promote the progress of the reaction, which will make the product obtained from the reaction mixed with a small amount of benzoic acid, making the post-processing complicated, and the amount of catalyst used is large, resulting in high production costs.

Method used

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  • The method for the synthesis of methyl benzoate by two still combined phase transfer catalysis
  • The method for the synthesis of methyl benzoate by two still combined phase transfer catalysis
  • The method for the synthesis of methyl benzoate by two still combined phase transfer catalysis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1, a kind of method that two kettles combine phase-transfer catalysis to synthesize methyl benzoate may further comprise the steps:

[0044] 1), add 24.4g (0.2mol) of benzoic acid, 9.2g (0.23mol) of sodium hydroxide, 60ml of water and 0.5 g (accounting for 2% of the mass of raw material benzoic acid), charged with excess methyl chloride (20.2g, 0.4mol), the temperature of the reaction solution in the control kettle was about 80°C, the reaction pressure was 2.3Mpa, and the reaction was carried out for 4h.

[0045] 2), benzoic acid 24.4g (0.2mol), sodium hydroxide 9.2g (0.23mol), 60ml water and tetrabutylammonium bromide 0.5g are housed in reaction kettle II (250mL autoclave) as reaction base material, That is, the consumption of benzoic acid, sodium hydroxide, water, phase-transfer catalyst in reactor II is the same as reactor I;

[0046] Step 1) after the reactor I reaction is finished, the gas in the reactor I is passed into the above reactor II while it is...

Embodiment 2

[0051] Embodiment 2, a kind of method that two still combined phase-transfer catalytic synthesis methyl benzoate comprises the following steps:

[0052] 1), add benzoic acid 24.4g (0.2mol), sodium hydroxide 9.2g (0.23mol), 60ml water and tetrabutylammonium iodide 0.4 g (accounting for 1.5% of the mass of raw material benzoic acid), charged with excess methyl chloride (20.2g, 0.4mol), controlled the temperature of the reaction solution in the kettle to be about 75°C, the reaction pressure was 2.0Mpa, and reacted for 6h.

[0053] 2), benzoic acid 24.4g (0.2mol), sodium hydroxide 9.2g (0.23mol), 60ml water and tetrabutylammonium iodide 0.4g are housed in reaction kettle II (250mL autoclave) as reaction bottom material, That is, the consumption of benzoic acid, sodium hydroxide, water, phase-transfer catalyst in reactor II is the same as reactor I;

[0054] Step 1) After the reaction in the reaction kettle I is completed, the gas in the reaction kettle I is passed into the above-...

Embodiment 3

[0059] Embodiment 3, a kind of method that two kettles combine phase-transfer catalysis to synthesize methyl benzoate, comprise the following steps:

[0060] 1), add benzoic acid 24.4g (0.2mol), sodium hydroxide 9.2g (0.23mol), 60ml water and tetraethylammonium bromide 5.6 g (accounting for 3% of the mass of raw material benzoic acid), charged with excess methyl chloride (20.2g, 0.4mol), the temperature of the reaction solution in the control kettle was about 70°C, the reaction pressure was 1.6Mpa, and the reaction was carried out for 6h.

[0061] 2), benzoic acid 24.4g (0.2mol), sodium hydroxide 9.2g (0.23mol), 60ml water and tetraethylammonium bromide 5.6g are housed in reaction kettle II (250mL autoclave) as reaction bottom material, That is, the consumption of benzoic acid, sodium hydroxide, water, phase-transfer catalyst in reactor II is the same as reactor I;

[0062] Step 1) After the reaction in the reaction kettle I is completed, the gas in the reaction kettle I is p...

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Abstract

The invention discloses a method of synthesizing methyl benzoate by two-kettle combined phase-transfer catalysis. The method comprises the following steps: 1) in a reaction kettle I, by taking benzoic acid, sodium hydroxide and chloromethane as raw materials, performing an esterification reaction in water under the action of a phase transfer catalyst; 2) filing benzoic acid, sodium hydroxide, water and a phase transfer catalyst in a reaction kettle II as a reaction primer, and after reaction of the reaction kettle I in the step 1), introducing gas in the reaction kettle I into the reaction kettle II while being hot to recover unreacted chloromethane, and continuously filing chloromethane into the reaction kettle II for the esterification reaction; 3) performing post treatment, namely dividing a reaction liquid after reaction in the reaction kettle I, and washing and distilling an organic phase at a reduced pressure with saturated edible salt water to obtain a product methyl benzoate; and 4) after the reaction in the reaction kettle II, and repeating the steps 2) and 3) after reaction in the reaction kettle I.

Description

technical field [0001] The invention relates to a method for preparing methyl benzoate from benzoic acid, sodium hydroxide and methyl chloride in the presence of a phase transfer catalyst. Background technique [0002] Methyl benzoate is an important fine chemical raw material. It can be used as a solvent for cellulose ester, cellulose ether, resin, rubber, etc. It can be used to prepare perfume essence and artificial essential oil, and it is also widely used as a food additive. [0003] The traditional production technology of methyl benzoate is to take the concentrated sulfuric acid as catalyzer, gained by the esterification of benzoic acid and methyl alcohol, and reaction formula is as follows: [0004] [0005] This method has the disadvantages of many side reactions, complicated product separation, serious equipment corrosion, and waste liquid polluting the environment. [0006] People such as Xu Qiu (Journal of Dalian Institute of Light Industry, 1995,14 (4): 23-27...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/10C07C69/78B01J19/18
CPCY02P20/584
Inventor 陈新志高武成牛石振钱超
Owner ZHEJIANG UNIV