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Method for preparing tert-butyl (meth)acrylate

A technology of tert-butyl acrylate and acrylic acid, applied in the field of preparation of tert-butyl acrylate, can solve the problems of small reaction space velocity, catalyst deactivation reaction selectivity, low activity and the like

Active Publication Date: 2019-09-24
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Another object of the present invention is to provide a kind of preparation method of tert-butyl (meth)acrylate, it not only has advantages such as simple process route, acid catalyst is nontoxic and harmless and production process is friendly to the environment, and the catalyzer that it uses overcomes The defects of low activity, small reaction space velocity, fast catalyst deactivation and insufficient reaction selectivity of existing catalysts are overcome, thereby advantageously reducing the production cost of tert-butyl acrylate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of catalyst

[0044] Weigh 53.8 grams of niobium oxalate and dissolve it in 1000ml of distilled water. After the niobium oxalate is completely dissolved, weigh 3.22 grams of zirconium oxychloride and add it to the solution. After it is completely dissolved, add 25% ammonia water dropwise until the pH of the solution is reached reach 8.0, filter and wash the precipitate with distilled water, then heat-treat at 500°C for 4 hours, add 20 grams of the treated solid into 10% sulfuric acid solution, stir at room temperature for 8 hours, then filter and wash the filter cake with distilled water, Then dry it in an oven at 110°C, shape the obtained solid into 10-20 mesh particles, and use it for the activity test.

[0045] Esterification reaction

[0046] The reaction of acrylic acid and isobutylene is carried out in a stainless steel tubular reactor, the volume of the solid acid catalyst prepared above is 20ml, the feed molar ratio of liquid phase acrylic acid ...

Embodiment 2

[0052] Using the same catalyst and activity testing method as in Example, but the volume space velocity of liquid isobutene was increased to 3.0 / h, the results are shown in the table below.

Embodiment 3

[0054] Using the same catalyst and activity testing method as in Example, but the volume space velocity of liquid isobutene was increased to 4.0 / h, the results are shown in the table below.

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PUM

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Abstract

The invention discloses a method for preparing tert-butyl (meth)acrylate. The method is characterized in that liquid acrylic acid and liquid isobutylene are mixed according to a molar ratio of 0.5:1.0 to 3.0:1.0, and then are reacted in a fixed bed tubular reactor, the reactor is filled with a niobium-zirconium composite oxide catalyst, and a molar ratio of niobium to zirconium in the niobium-zirconium composite oxide is 1:(0.01-2).

Description

technical field [0001] The invention relates to a preparation method of tert-butyl (meth)acrylate. The method of the invention not only has the advantages of simple process route, non-toxic and harmless acid catalyst, and environment-friendly production process, but also the catalyst used overcomes the low activity, small reaction space velocity, fast catalyst deactivation and reaction of existing catalysts. The defect of insufficient selectivity, thereby advantageously reducing the production cost of tert-butyl acrylate. Background technique [0002] Tert-butyl acrylate is an important organic acid ester. It is a colorless and transparent liquid at room temperature. It has good chemical and physical properties such as weather resistance, water resistance, oil resistance, and chemical resistance. Because of its unique and highly active unsaturated double bond and carboxylic acid (-COOR) structure, many kinds of polymer formulations with good performance can be derived, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/20B01J37/03B01J37/08C07C67/08C07C67/04C07C69/54
CPCB01J23/20B01J23/002B01J37/031B01J37/088C07C67/08C07C67/04C07C69/54Y02P20/584
Inventor 熊德胜颜建龙王懿斌庄岩吴通好马建学钱志刚褚小东
Owner SHANGHAI HUAYI NEW MATERIAL
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