Method for preparing methyl p-tert-butylbenzoate

A technology for methyl tert-butyl benzoate and tert-butyl benzoic acid, applied in the field of preparing methyl tert-butyl benzoate, can solve the problems of large environmental pollution, easy water loss of organic matter, easy hydrolysis of catalysts, etc. Environmentally friendly, easy to industrialize, easy to separate

Active Publication Date: 2017-11-03
BEIJING INSTITUTE OF TECHNOLOGYGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional synthetic method of methyl p-tert-butylbenzoate is to use concentrated sulfuric acid as a catalyst to directly catalyze the esterification reaction. Although the yield is high, the organic matter is prone to dehydration and carbonization, and the reaction time is long, and it is difficult to process after separation.
Moreover, this method has a great impact on environmental pollution, and its waste water discharge is large, which seriously corrodes the equipment.
Another method is usually to use anhydrous AlCl 3 , FeCl 3 , titanium sulfate is used as catalyst to synthesize methyl p-tert-butylbenzoate. This method needs to adopt the distillation water separation process to control the reflux reaction. Although the conversion rate is high and the operation is simple, the catalyst used in this method is easy to hydrolyze, and the reaction needs to be strictly controlled. Carried out under anhydrous conditions, and continuous water separation is required during the reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add the raw materials of methanol and p-tert-butylbenzoic acid with a molar ratio of 10:1 into the reactor, then add a polystyrene sulfonic acid resin catalyst with a raw material weight percentage of 10%, heat, and at a reaction temperature of 100°C, the reaction pressure Under the condition of 1Mpa, stir to carry out the esterification reaction. After reacting for 8 hours, the reaction solution was discharged and centrifuged, and the obtained upper product was the crude product of methyl p-tert-butylbenzoate, water and a small amount of raw materials p-tert-butylbenzoic acid and methanol, and the upper product was rotary-evaporated to remove methanol , water, and then rotary steaming to obtain the target product methyl p-tert-butylbenzoate, wherein unreacted p-tert-butylbenzoic acid and methanol are recycled, and the lower layer catalyst is recycled. The yield of methyl p-tert-butylbenzoate is 95%, and the purity is more than or equal to 99.99%.

Embodiment 2

[0034] Add the raw materials of methanol and p-tert-butylbenzoic acid with a molar ratio of 10:1 into the reactor, and then add a perfluorosulfonic acid resin catalyst with a raw material weight percentage of 10%, and heat it at a reaction temperature of 120°C and a reaction pressure of 1.5 Under the condition of Mpa, stir, carry out esterification reaction. After reacting for 5 hours, the reaction solution was discharged and centrifuged, and the obtained upper product was the crude product of methyl p-tert-butylbenzoate, water and a small amount of raw materials p-tert-butylbenzoic acid and methanol, and the upper product was rotary-evaporated to remove methanol , water, and then rotary steaming to obtain the target product methyl p-tert-butylbenzoate, wherein unreacted p-tert-butylbenzoic acid and methanol are recycled, and the lower layer catalyst is recycled. The yield of methyl p-tert-butylbenzoate is 96%, and the purity is more than or equal to 99.99%.

Embodiment 3

[0036] Add the raw materials of methanol and p-tert-butylbenzoic acid with a molar ratio of 10:1 into the reactor, then add a polystyrenesulfonic acid resin catalyst with a raw material weight percentage of 15%, heat, and at a reaction temperature of 120°C, a reaction pressure of Under the condition of 1.5Mpa, stir to carry out esterification reaction. After reacting for 3 hours, the reaction liquid was discharged and centrifuged, and the obtained upper product was the crude product of methyl p-tert-butylbenzoate, water and a small amount of raw materials p-tert-butylbenzoic acid and methanol, and the upper product was rotary-evaporated to remove methanol , water, and then rotary steaming to obtain the target product methyl p-tert-butylbenzoate, wherein unreacted p-tert-butylbenzoic acid and methanol are recycled, and the lower layer catalyst is recycled. The yield of methyl p-tert-butylbenzoate is 94%, and the purity is more than or equal to 99.99%.

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Abstract

The invention relates to a method for preparing methyl p-tert-butylbenzoate. The method comprises the following steps: with methanol and p-tert-butyl benzoic acid as raw materials, under the action of sulfonic acid resin as a catalyst, performing an esterification reaction, and separating to obtain the methyl p-tert-butylbenzoate, wherein the sulfonic acid resin as the catalyst is environment-friendly, can be easily separated from a product and can be recycled. The method has the advantages as follows: the catalyst is good in stability, high in reactivity and environment-friendly, equipment corrosion is avoided, the product is easy to separate, and the catalyst can be recycled.

Description

technical field [0001] The invention relates to a method for preparing methyl p-tert-butylbenzoate, in particular to a method for preparing methyl p-tert-butylbenzoate under the action of a green acid catalyst. Background technique [0002] As an important organic synthesis intermediate and pharmaceutical intermediate, methyl p-tert-butylbenzoate is widely used in chemical synthesis, cosmetics, pharmaceuticals, flavors and fragrances and other industries. The annual demand of the market is very large, therefore, research on the synthesis of methyl p-tert-butylbenzoate has important value. [0003] The production method of methyl p-tert-butylbenzoate is mainly to produce p-tert-butylbenzoic acid and methanol through the esterification reaction under the catalysis of an acid catalyst. The traditional synthetic method of methyl p-tert-butylbenzoate is to use concentrated sulfuric acid as a catalyst to directly catalyze the esterification reaction. Although the yield is high, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/76C07C67/08
CPCC07C67/08C07C69/76Y02P20/584
Inventor 吴芹黎汉生周广增宋淑芬任荣史大昕成金玉
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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