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High-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation method

A technology of tetrachlorobenzoyl and tetrachlorophthalic anhydride, which is applied in the field of high-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation, can solve problems such as unstable yield, and achieves The effect of increasing yield, reducing environmental pollution and material waste

Pending Publication Date: 2017-12-01
江苏万隆化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But in existing production technology, the yield of 2,3,4,5-tetrachlorobenzoyl chloride is unstable all the time, how to develop the synthetic technique that yield is higher and reaction is more stable is modern 2,3,4,5- An important direction for the production of tetrachlorobenzoyl chloride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A high-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation method, characterized in that the preparation method is:

[0021] 1. Add 150g of tetrachlorophthalic anhydride, 35g of sodium hydroxide, and 600g of distilled water into the autoclave to keep the pressure inside the autoclave at 15Kg / cm 2 , carry out stirring and heat up to 180°C, the stirring speed is 75r / min, and after reacting at this temperature and pressure for 10h, the temperature is lowered to normal temperature, and the reaction product is pressed out of the reactor;

[0022] 2. The reaction product obtained in step 1 is adjusted to PH=1 with hydrochloric acid, wherein the concentration of hydrochloric acid is 15%, and when the white solid no longer precipitates, carry out suction filtration, clear water washing, and drying to obtain solid products 2, 3, and 4 , 5-tetrachlorobenzoic acid;

[0023] 3. Weigh 100 g of the solid product 2,3,4,5-tetrachlorobenzoic acid obtained in step 2 and add to the rea...

Embodiment 2

[0026] A high-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation method, characterized in that the preparation method is:

[0027] 1. Add 150g of tetrachlorophthalic anhydride, 35g of potassium hydroxide, and 600g of distilled water into the autoclave to keep the pressure inside the autoclave at 18Kg / cm 2 , stirring to raise the temperature to 190°C, the stirring speed is 75r / min, and after reacting for 10h under the temperature and pressure conditions, the temperature is lowered to normal temperature, and the reaction product is pressed out of the reactor;

[0028] 2. Adjust the pH of the reaction product obtained in step 1 to 1 with hydrochloric acid, wherein the concentration of hydrochloric acid is 8%, and when the white solid no longer precipitates, carry out suction filtration, clear water washing, and drying to obtain solid products 2, 3, and 4 , 5-tetrachlorobenzoic acid;

[0029] 3. Weigh 100 g of the solid product 2,3,4,5-tetrachlorobenzoic acid obtained in step ...

Embodiment 3

[0032] A high-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation method, characterized in that the preparation method is:

[0033] 1. Add 150g of tetrachlorophthalic anhydride, 35g of potassium carbonate, and 600g of distilled water into the autoclave to keep the pressure inside the autoclave at 20Kg / cm 2 , stirring to raise the temperature to 200°C, with a stirring speed of 75r / min, and reacting at this temperature and pressure for 10 hours, then lowering the temperature to normal temperature, and pressing the reaction product out of the reactor;

[0034] 2. The reaction product obtained in step 1 is adjusted to PH=1 with hydrochloric acid, wherein the concentration of hydrochloric acid is 35%, and when the white solid no longer precipitates, carry out suction filtration, clear water washing, and drying to obtain solid products 2, 3, and 4 , 5-tetrachlorobenzoic acid;

[0035] 3. Weigh 100 g of the solid product 2,3,4,5-tetrachlorobenzoic acid obtained in step 2 and add t...

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PUM

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Abstract

The invention discloses a high-yield 2,3,4,5-tetrachlorobenzoyl chloride preparation method. 2,3,4,5-tetrachlorobenzoic acid is firstly prepared from tetrachlorophthalic anhydride used as a raw material, then the final product 2,3,4,5-tetrachlorobenzoyl chloride is prepared with a reflux reaction method, specific temperature and pressure increase or a closed reflux reaction is adopted according to the reaction characteristic in the reaction process, the yield of the final product is ensured to be increased remarkably, a catalyst and a solvent in the reaction are recovered, environmental pollution and material waste are reduced, and a contribution is made to energy saving and environmental protection.

Description

technical field [0001] The invention relates to a manufacturing method of chemical raw materials and chemical products for pharmaceutical intermediates in the manufacturing of chemical products, in particular to a method for preparing high-yield 2,3,4,5-tetrachlorobenzoyl chloride. Background technique [0002] The development of modern medicine has a history of more than 100 years. After the middle of the 19th century, due to the development of organic synthesis and chemical industry, the production of drugs has the original synthesis of active ingredients extracted from natural plants for industrial purposes, forming the first development. It can be said that the development of the chemical and pharmaceutical industry was in its infancy at the end of the 19th century, and it had begun to take shape. In the 1930s, the advent of sulfonamides set a new milestone in chemotherapy and enabled the modern pharmaceutical industry to develop more rapidly. Since then, the pharmaceut...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C51/64C07C63/70C07C51/087C07C51/38C07C63/68C07C51/41
CPCC07C51/087C07C51/38C07C51/412C07C51/60C07C51/64C07C63/70C07C63/68
Inventor 郁红明
Owner 江苏万隆化学有限公司