Preparation process for catalyzing and synthesizing tert-butyl acrylate by using strong acid cation exchange resin as catalyst

A strong acidic cation and tert-butyl acrylate technology, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, organic chemistry, etc., can solve the problems of product tert-butyl acrylate decomposition, difficult distillation of target products, and increase of by-products, etc. , achieve the effects of simplified steps, excellent low-temperature reactivity and selectivity, and resource saving

Active Publication Date: 2013-05-01
山东敏德化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the catalyst, product and remaining raw materials are separated after the esterification reaction, the catalyst will be washed out together with water to form a large amount of waste acid and waste water, which will pollute the environment; at the same time, these strongly acidic homogeneous catalysts are difficult to be recovered after the reaction is completed. Completely neutralized and washed out, resulting in the decomposition of the product tert-butyl acrylate in the rectification process
Catalytic synthesis of gas and liquid will increase energy consumption and increase by-products, which will bring difficulty to the rectification of target products in the later stage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of preparation technology that takes strongly acidic cation exchange resin as catalyst to catalyze the synthesis of tert-butyl acrylate is carried out successively according to the following steps:

[0029] 1) Add acrylic acid, strongly acidic cation exchange resin, polymerization inhibitor A, and polymerization inhibitor B in parts by mass of 280 parts, 20 parts, 10 parts, and 1 part respectively into a closed reaction kettle, and add the parts by mass drop by drop Carry out esterification reaction for 300 parts of liquefied isobutylene, add dropwise for 1.5 hours, during which the temperature is kept at -20°C; polymerization inhibitor A is an ether type polymerization inhibitor, and polymerization inhibitor B is a phenol type polymerization inhibitor;

[0030] The reaction formula is:

[0031] + →

[0032] 2) After the dropwise addition is completed, keep warm at -20°C for 6 hours;

[0033] 3) After the heat preservation is completed, the closed react...

Embodiment 2

[0037] The difference with embodiment 1 is:

[0038] The mass parts of acrylic acid, strongly acidic cation exchange resin, polymerization inhibitor A, polymerization inhibitor B, and liquefied isobutylene are respectively 320 parts, 35 parts, 20 parts, 5 parts, 430 parts;

[0039] The dropping time is 3 hours, and the esterification reaction temperature is kept at 10°C;

[0040] After the dropwise addition is completed, keep warm at 10°C for 7 hours;

[0041] The mass fraction of the obtained tert-butyl acrylate was 450 parts, and the yield was 99.7%.

Embodiment 3

[0043] The difference with embodiment 1 is:

[0044] 1) The mass parts of acrylic acid, strongly acidic cation exchange resin, polymerization inhibitor A, polymerization inhibitor B, and liquefied isobutylene are 360 ​​parts, 50 parts, 30 parts, 10 parts and 560 parts respectively;

[0045] 2) The dropping time is 4 hours, and the esterification reaction temperature is kept at 40°C;

[0046] 3) After the dropwise addition is completed, keep warm at 40°C for 8 hours;

[0047] 4) The mass fraction of the prepared tert-butyl acrylate is 780 parts, and the yield is 99.8%.

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Abstract

The invention discloses a preparation process for catalyzing and synthesizing tert-butyl acrylate by using strong acid cation exchange resin as a catalyst, belonging to the technical field of organic synthesis. The preparation process is characterized by comprising the steps of: adding crylic acid, strong acid cation exchange resin, a polymerization inhibitor A and a polymerization inhibitor B into a closed reaction kettle, dropwise adding liquefied isobutene for carrying out esterification reaction; after dropwise adding is completed, carrying out thermal insulation; after the thermal insulation is finished, releasing the pressure of the closed reaction kettle, filtering, extracting a liquid component to enter a rectifying tower; and sequentially separating byproducts of tertiary butanol and diisobutylene and a target project of the tert-butyl acrylate. The preparation process has the beneficial effects that the liquefied isobutene is adopted to be directly catalyzed together with the crylic acid and the cation exchange resin under the action of the polymerization inhibitor A and the polymerization inhibitor B to form a specific catalysis system, gaseous isobutene is not needed to be dissolved in a solvent containing crylic acid for carrying out esterification reaction under the action of the catalyst, and thus the procedure of absorbing a solvent in subsequent operation is removed, resources are saved and procedures are saved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation process of tert-butyl acrylate. Background technique [0002] Tert-butyl acrylate, its structural formula is . Tert-butyl acrylate is an extremely important chemical basic raw material and intermediate. Because of its unique and highly active polar molecule, unsaturated double bond and carboxylate (-COOR) structure, it can be derived into many kinds It has a polymer formula with good performance, and can prepare plastic, cross-linked and other polymers through emulsion polymerization, solution polymerization, copolymerization and other processing methods. [0003] In the PCT invention patent application document with the application number 20068001094.7, a method for synthesizing tert-butyl (meth)acrylate is described. In this method, a solid acid such as sulfuric acid is used as a catalyst, and tert-butanol is dehydrated to obtain gaseous i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/04
Inventor 徐德良丁峰孙迎河毕研飞王少东
Owner 山东敏德化工有限公司
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