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Method for continuously preparing carboxylic acid ester

A technology of carboxylate and carboxylic acid, which is applied in the field of continuous preparation of carboxylate, can solve the problems of time-consuming, short active operation cycle, low reactivity pollution rate, etc., and achieve the effect of simple method and short purification time

Inactive Publication Date: 2013-11-13
CHINA PETROCHEM DEVMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalyst can reduce the corrosion of equipment and environmental pollution, the preparation of the catalyst is cumbersome and the active operation cycle is short, and the esterification rate is lower than 90%, which is not in line with economic benefits.
[0007] CN 100503043C discloses an ionic liquid catalyst for esterification reaction and its preparation method and application. Although the ionic liquid has the advantages of high reactivity and low environmental pollution rate, the esterification catalytic effect is 2 to 12 hours. And after the reaction is over, it needs to stand still to separate the esterified product and the ionic liquid catalyst by gravity sedimentation, so it is more time-consuming to carry out the esterification reaction and separate and purify the esterified product
[0008] In summary, in order to improve the esterification rate of the traditional industrial esterification reaction, the use of concentrated sulfuric acid as a catalyst has the disadvantages of equipment corrosion and environmental pollution.

Method used

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  • Method for continuously preparing carboxylic acid ester
  • Method for continuously preparing carboxylic acid ester
  • Method for continuously preparing carboxylic acid ester

Examples

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preparation example Construction

[0019] In the preparation method of the present invention, if the carboxylic acid used is a monocarboxylic acid, the weight ratio of the monocarboxylic acid and alcohol required for the esterification reaction is 1:1 to 1:6, which can be used in the batching tank to The unit carboxylic acid (monocarboxylic acid) and alcohol are mixed at a temperature of 30°C to 80°C, and fed from below the vertical reactor at a rate of 1 to 12 LHSV per hour, and the esterification reaction is carried out at a temperature of 110°C to 190°C.

[0020] In another preparation method of the present invention, if the carboxylic acid used is a dibasic carboxylic acid, the weight ratio of the dibasic carboxylic acid and alcohol required for the esterification reaction is 1:3 to 1:10, which can be preceded by The dibasic carboxylic acid and alcohol are mixed at a temperature of 50°C to 75°C in the batching tank, fed from the bottom of the vertical reactor at 2 to 18 LHSV per hour, and esterified at a tem...

Embodiment 1

[0028] Acetic acid and absolute ethanol with a weight ratio of 1:2 or 1:3 were uniformly mixed in a batching tank at 30°C, and then fed from the bottom of the vertical reactor at 3LHSV per hour for reaction, and the reaction temperature was 115°C. The esterification mixture flows out from the upper outlet of the vertical reactor, is collected in a liquid collection bottle and analyzed by a gas chromatograph, and the acid value is determined by titration. The results of conversion and selectivity are listed in Table 1.

Embodiment 2 to 3

[0030] Repeat the operation mode of Example 1, according to the weight ratio shown in Table 1, the carboxylic acid and alcohol are uniformly mixed in the batching tank at 30 ° C, and according to Table 1, they are fed into the reactor from the bottom of the vertical reactor at different speeds, According to Table 1, the reactions were carried out at different reaction temperatures. The measurement results of conversion and selectivity are listed in Table 1.

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Abstract

A method for continuously preparing a carboxylic acid ester is disclosed. In the method of the present invention, a vertical reactor is filled with a solid catalyst, a carboxylic acid and an alcohol are introduced into a lower part of the vertical reactor, esterification is performed to form an esterized mixture, the esterized mixture is output from an upper part of the vertical reactor, and distillation is performed to isolate the carboxylic acid ester. The method of the present invention is simple, easily controlled and environmental friendly, and has significantly high conversion rate and selectivity.

Description

technical field [0001] The present invention relates to a method for continuously preparing carboxylate, in more detail, relates to a method for continuously preparing carboxylate through the esterification reaction of carboxylic acid and alcohol. Background technique [0002] Carboxylate is an important fine chemical product, which has the characteristics of good solubility, easy flow, safety and non-toxicity, photochemical stability, etc., so that it can not only be used as a raw material for organic synthesis, but also an important fine chemical product, widely used in cold resistance Organic synthesis industries such as plasticizers, solvents, tobacco, spices, flavors, cosmetics, medicines, coatings, surfactants, rubber and plastics, polyester resins, adhesives, synthetic fibers, and film materials. [0003] Carboxylate compounds in traditional industries use heating or acid catalysis to carry out esterification reaction between carboxylic acid and alcohol. The esterific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08
CPCC07C67/08C07C69/14C07C69/24C07C69/54C07C69/78C07C69/44C07C69/42C07C69/40C07C69/50C07C69/60C07C69/80C07C69/007
Inventor 黄志达龚永顺蔡耀庆
Owner CHINA PETROCHEM DEVMENT
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