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Method of preparing acryloyl chloride by virtue of continuous method

An acryloyl chloride, continuous process technology, applied in the chemical industry, can solve the problems of complex acryloyl chloride process, product purity, low yield, etc., and achieve the effect of significant technological progress and quality improvement.

Inactive Publication Date: 2015-05-06
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In view of the above-mentioned defects in the prior art, the technical problem to be solved by the present invention is to provide a method for preparing acryloyl chloride by a continuous method, and the method for preparing acryloyl chloride by a continuous method should solve the problem of preparing acryloyl chloride in the prior art. The process of acid chloride is complicated, and the technical problems of product purity and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] First, add 250 mL of acrylic acid and 2.0 g of polymerization inhibitor to a 500 mL four-necked flask equipped with a thermometer, agitator, a constant pressure dropping funnel and a distillation system (including a distillation head, a straight condenser tube and a collection bottle), and stir. When heated to 85°C / 200mmHg at low temperature, 250g thionyl chloride (purity greater than 95%) and 150g acrylic acid (purity greater than 99%) were added dropwise. At the same time, acryloyl chloride is collected by distillation, and the yield of acryloyl chloride in terms of thionyl chloride reaches 86% (the reaction of thionyl chloride and acrylic acid is carried out by equimolar, and in this reaction, acrylic acid is excessive, so When calculating the yield of the product acryloyl chloride, that is, the yield, the input amount of thionyl chloride should be calculated.). (Note: This device is a reactor that integrates reaction and distillation. The temperature of the cooling ...

Embodiment 2

[0016] First, add 250 mL of acrylic acid and 2.0 g of polymerization inhibitor into a 500 mL four-necked flask equipped with a thermometer, agitator, a constant pressure dropping funnel and a distillation system. When heated to 85°C / 300 mmHg with stirring, add 250 g of chlorine dropwise. sulfoxide (purity greater than 95%) and 150 g acrylic acid (purity greater than 99%). Meanwhile, acryloyl chloride is collected by distillation, and its yield is 75-80% in terms of thionyl chloride.

Embodiment 3

[0018] First, add 250 mL of acrylic acid and 2.0 g of polymerization inhibitor into a 500 mL four-necked flask with a thermometer, a stirrer, a constant-pressure dropping funnel and a distillation system. When heated to 85°C / 500 mmHg with stirring, add 250 g of chlorine dropwise. sulfoxide (purity greater than 95%) and 150 g acrylic acid (purity greater than 99%). At the same time, acryloyl chloride is collected by distillation, and its yield is less than 50% in terms of thionyl chloride.

[0019] The boiling point of acryloyl chloride under normal pressure is 72°C. The higher the vacuum degree, the lower the boiling point. In Examples 2 and 3, the degree of vacuum is relatively higher than that in Example 1, so that once the acryloyl chloride is generated, the boiling point of the distilled acryloyl chloride is low, the temperature difference between it and the cooling liquid is small, it is not easy to cool, and a large amount of propylene The acyl chloride is pumped into t...

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PUM

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Abstract

The invention discloses a method of preparing acryloyl chloride by virtue of a continuous method. The method comprises the following steps: respectively weighing a first batch of acrylic acid mass and inhibitor mass as well as a second batch of acrylic acid mass and inhibitor mass, wherein the mass of the inhibitor accounts 0.5-1.0 percent of the mass of acrylic acid in the first batch; then adding the first batch of acrylic acid into a reaction vessel, adding the inhibitor, stirring at 200-250rap / min, heating to 78-88 DEG C / 200-500mm Hg, then adding the second batch of acrylic acid and thionyl chloride, cooling acryloyl chloride generated by reaction by virtue of a condenser, and collecting acryloyl chloride under reduced pressure of 200-500mmHg. According to the method disclosed by the invention, at certain temperature and pressure, acryloyl chloride is collected while the materials are fed, so that the phenomenon that the side reactions including polymerization and addition are easily caused when a target product stays in a reaction system with relatively high temperature for a long time is avoided, the quality of the product is greatly improved, and the yield of the product is greatly increased.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to acryloyl chloride, in particular to a continuous method for preparing acryloyl chloride. Background technique [0002] Acryloyl chloride is active in chemical properties and can undergo various chemical reactions. It is an important intermediate in organic synthesis. It is mainly used to prepare special acrylate products and acrylamide products. In recent years, some people have used acryloyl chloride and polyether to prepare polymer membrane materials. The existing continuous method for preparing acryloyl chloride has a low yield and purity of acryloyl chloride, and the follow-up process is cumbersome. Therefore, there are few processes for industrially preparing acryloyl chloride at present. Contents of the invention [0003] In view of the above-mentioned defects in the prior art, the technical problem to be solved by the present invention is to provide a method...

Claims

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Application Information

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IPC IPC(8): C07C57/04C07C51/60
CPCC07C51/60
Inventor 金东元
Owner SHANGHAI INSTITUTE OF TECHNOLOGY