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Synthesis method of photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone

A photoinitiator and synthesis method technology, applied in the chemical field, can solve the problems of environmental pollution, low yield, waste water and waste gas, etc., and achieve the effects of high yield, increased product content, and less pollution

Active Publication Date: 2014-03-05
岳阳市国发植物用药工程技术研究中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production process of 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone is mainly based on acid chloride reaction between isobutyric acid and phosphorus trichloride or thionyl chloride. The defect is that the production process produces More by-products such as phosphoric acid or sulfur dioxide, more waste water and waste gas, easy to pollute the environment, and the yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Put 1500kg of isobutyric acid into the reactor, raise the temperature to 40-45°C, feed phosgene, the phosgene (volume) content is ≥90%, the pressure is 0.05MPa, and the flow rate is 40m 3 / h, light transmission 650m 3 , kept at 48-51°C for 2 hours, sampling and analysis did not contain isobutyric acid, the content was 99.26% isobutyryl chloride 1780kg, and the yield was 95.64%. The molar ratio of the amount of phosgene introduced to the isobutyric acid fed is 1.1:1.

[0027] 2. Put the metered amount of pure benzene and the quantitative catalyst aluminum trichloride into the reaction kettle, lower the temperature, and add isobutyryl chloride dropwise at a temperature below 10°C, and keep the temperature at 8-15°C for 3 hours to obtain 2-methyl-1-phenyl-1 -Aluminum trichloride complex of propyl ketone. The molar ratio of pure benzene, aluminum trichloride and isobutyryl chloride is 3.05:1:1.

[0028] 3. Put the measured amount of 2-methyl-1-phenyl-1-propyl ketone ...

Embodiment 2

[0033]1. Put 1550kg of isobutyric acid into the reactor, raise the temperature to 45-50°C, and feed phosgene. The phosgene (volume) content is ≥90%, the pressure is 0.08MPa, and the flow rate is 45m 3 / h, light transmission 680m 3 , kept at 48-51°C for 2 hours, sampled and analyzed without isobutyric acid, the content was 99.31% isobutyryl chloride 1797kg, and the yield was 96.57%. The molar ratio of the amount of phosgene introduced to the isobutyric acid fed is 1.2:1.

[0034] 2. Put the metered amount of pure benzene and the quantitative catalyst aluminum trichloride into the reaction kettle, lower the temperature, and add isobutyryl chloride dropwise at a temperature below 10°C, and keep the temperature at 8-15°C for 3 hours to obtain 2-methyl-1-phenyl-1 -Aluminum trichloride complex of propyl ketone. The molar ratio of pure benzene, aluminum trichloride and isobutyryl chloride is 3.1:1:1.

[0035] 3. Put the measured amount of 2-methyl-1-phenyl-1-propyl ketone aluminu...

Embodiment 3

[0040] 1. Put 1600kg of isobutyric acid into the reactor, raise the temperature to 45-50°C, and feed phosgene, the content of phosgene (volume) is ≥90%, the pressure is 0.1MPa, and the flow rate is 50m 3 / h, light transmission 700m 3 , kept at 48-51°C for 2 hours, sampling and analysis did not contain isobutyric acid, the content was 99.07% after analysis and 1789kg of isobutyryl chloride was obtained, and the yield was 96.13%. The molar ratio of the amount of phosgene introduced to the isobutyric acid fed is 1.3:1.

[0041] 2. Put the metered amount of pure benzene and the quantitative catalyst aluminum trichloride into the reaction kettle, lower the temperature, and add isobutyryl chloride dropwise at a temperature below 10°C, and keep the temperature at 8-15°C for 3 hours to obtain 2-methyl-1-phenyl-1 -Aluminum trichloride complex of propyl ketone. The molar ratio of pure benzene, aluminum trichloride and isobutyryl chloride is 3.15:1:1.

[0042] 3. Put the measured amo...

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Abstract

The invention relates to a synthesis method of a photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone, which comprises the following steps: reacting high-purity gas phosgene with isobutyric acid to synthesize isobutyryl chloride; and carrying out chlorine substitution reaction by a cascade technique: exhaust of a first reaction kettle after chlorine introduction is connected into a second reaction kettle in cascade, and hydrogen chloride and chlorine in the exhaust released by the first reaction enter the second reaction kettle to catalyze the absorption and utilization. The method can well enhance the purity of isobutyryl chloride and further enhance the purity and yield of the product 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone; and the catalytic action of hydrogen chloride in the exhaust is utilized to increase the reaction speed, lower the chlorine consumption and enhance the product content. The generated exhaust is recycled after innocent treatment, thereby solving the problem of environmental pollution of the exhaust.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a method for synthesizing photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-propyl ketone. First, high-purity gaseous phosgene and isobutyric acid are used to react and synthesize isobutyl Acyl chloride; in the chlorine substitution reaction, a series process is adopted. The tail gas after the first reactor is connected to the second reactor in series, and the tail gas released by the first reaction is hydrogen chloride and chlorine, which enters the second reactor to catalyze and Absorb and utilize. This method can improve the purity of isobutyryl chloride well, and further improve the purity and the yield of product 2-hydroxyl-2-methyl-1-phenyl-1-propyl ketone, while utilizing the catalysis of hydrogen chloride in the tail gas, The reaction speed is accelerated, the consumption of chlorine gas is reduced, and the product content is increased. The generated tail gas is recovered thro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/82C07C45/64
CPCC07C45/46C07C45/63C07C45/64C07C51/60C07C49/82C07C49/80C07C49/76C07C53/42
Inventor 胡晓珊陈珍李国栋刘春国黎辉良李契
Owner 岳阳市国发植物用药工程技术研究中心有限公司
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