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Methyl benzoate preparation method

A technology of methyl benzoate and benzoic acid, which is applied in the field of preparation of methyl benzoate, can solve the problems of frequent regeneration, high price, complex preparation process of solid catalyst, etc., achieve less by-products, high recycling performance, and optimize ester chemical reaction effect

Inactive Publication Date: 2019-04-30
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of solid catalyst is complex, expensive, and requires frequent regeneration during the production process

Method used

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  • Methyl benzoate preparation method
  • Methyl benzoate preparation method
  • Methyl benzoate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1 Preparation of quaternary phosphonium salt ionic liquid catalyst

[0016] The quaternary phosphonium salt ionic liquid used in the present invention is prepared according to the following steps: under ion exchange reaction conditions, the first quaternary phosphonium salt is contacted with a protonic acid to obtain a contact product. Wherein, the general formula of the first quaternary phosphonium salt is [Bu 3 PR] + Z - , R is C 6 -C 16 straight-chain or branched-chain alkyl, and Z is halogen. The general formula of a protic acid is H + x - , X - selected from p-C 7 h 7 SO 3 - 、CF 3 SO 3 - 、HSO 4 - and H 2 PO 4 - at least one of the The first quaternary phosphonium salt can be obtained commercially, and can also be prepared by methods well known to those skilled in the art. The first quaternary phosphonium salt includes but is not limited to [Bu 3 PC 12 h 25 ] + Cl - 、[Bu 3 PC 14 h 29 ] + C - 、[Bu 3 PC 10 h 21 ] + Cl - a...

Embodiment 2

[0019] The preparation of embodiment 2 methyl benzoate

[0020] ⑴Esterification reaction: add 61.73 benzoic acid, 80.96g methanol and 7.14g quaternary phosphonium salt ionic liquid in 500ml autoclave (the molar ratio of benzoic acid and methanol is 1:5, quaternary phosphonium salt ionic liquid 5% (weight) of the weight, the quaternary phosphonium salt ionic liquid is [Bu 3 PC 14 h 29 ] + [p-C 7 h 7 SO 3 ] - . Start stirring (350 rpm), then start heating, bring the temperature in the autoclave to 130°C, start timing, and react for 3 hours;

[0021] (2) Separation and purification of methyl benzoate: ① After the reaction, turn off the heating power supply, and after cooling down to room temperature, stop stirring, transfer the reaction solution to a distillation device (normal pressure), heat up, and distill to evaporate unreacted methanol. ② After no methanol is evaporated, turn off the heating, lower the temperature, change the atmospheric distillation device to a red...

Embodiment 3

[0024] The preparation of embodiment 3 methyl benzoate

[0025] (1) Esterification reaction: Add 54.05 g of benzoic acid, 70.88 g of methanol and 24.99 g of quaternary phosphonium salt ionic liquid in a 500ml autoclave (the molar ratio of benzoic acid and methanol is 1:5, and the quaternary phosphonium salt ionic liquid catalyst is the total reactant 20% (weight) of the weight, the quaternary phosphonium salt ionic liquid is [Bu 3 PC14 h 29 ] + [p-C 7 h 7 SO 3 ] - . Start stirring (350 rpm), then start heating, bring the temperature in the autoclave to 130°C, start timing, and react for 3 hours;

[0026] (2) separation and purification of methyl benzoate: method of operation and steps are with embodiment 2, collect cut 44.37g altogether;

[0027] (3) Analysis and detection: the cut obtained by distillation under reduced pressure, i.e. methyl benzoate sampling is carried out by gas chromatography, with a purity of 99.6%;

[0028] The calculated yield of methyl benzoate...

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Abstract

The invention relates to a methyl benzoate preparation method, which comprises: placing benzoic acid, methanol and a catalyst into a reactor, carrying out an esterification reaction, separating, and purifying to obtain methyl benzoate, wherein the catalyst is a quaternary phosphonium salt ionic liquid catalyst, the quaternary phosphonium salt ionic liquid has a general formula of [Bu3PR]<+>X<->, Ris C6-C16 linear alkyl, cycloalkyl or isomeric alkyl, and X<-> is p-C7H7SO3<->, CF3SO3<->, HSO4<-> or H2PO4<->. According to the present invention, the methyl benzoate is generated by carrying out the esterification reaction with the quaternary phosphonium salt ionic liquid catalyst, such that the effect of the esterification reaction is optimized, the activity of the catalyst is high, the by-products are few, the recycling performance is high, the selectivity and the yield of the product are easily improved, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical preparation, and relates to a preparation method of methyl benzoate. Background technique [0002] Methyl benzoate, chemically can be regarded as the product of alcoholysis of benzoic acid or benzoic anhydride or benzoyl chloride with methanol. Colorless transparent liquid. Miscible with methanol, ethanol, ether. Insoluble in water. Industrially, it can be used as an organic synthesis intermediate, solvent, and fragrance. It has a strong aroma of wintergreen oil and yunanga oil, and is used in the preparation of perfume essences and artificial essential oils, and is also widely used in food. [0003] The method for industrially synthesizing methyl benzoate mainly adopts concentrated sulfuric acid as a catalyst, and is prepared by the reaction of benzoic acid and methanol. This process route has many by-products, high corrosiveness, complicated product separation process, and environmental pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/78B01J31/02
CPCB01J31/0288B01J2231/49C07C67/08C07C69/78
Inventor 王仲霞王志侃陈春凤李华强赵军
Owner CHINA PETROLEUM & CHEM CORP
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