Preparation method of parachlorobenzoyl chloride

A technology of p-chlorobenzoyl chloride and p-chlorotoluene, which is applied in the field of preparation of p-chlorobenzoyl chloride, can solve the problems of many reaction side reactions, many impurities, and low product yield, and achieve short chlorination time and high yield , The effect of less reaction by-products

Inactive Publication Date: 2017-11-24
山东福尔有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this preparation method: 1, the chlorination reaction time ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Chlorination:

[0019] Add 3400kg p-chlorotoluene and 95kg thionyl chloride to the reactor, add 0.085kg triethanolamine and heat up to 85°C;

[0020] Weigh 20kg of azobisisobutyronitrile, add 0.5kg to the system first, and gradually add the remaining azobisisobutyronitrile during the reaction;

[0021] After being measured by the electronic scale of the liquid chlorine cylinder, the chlorine gas enters the liquid chlorine vaporizer through the liquid phase tube, is heated by the hot water in the vaporizer, and enters the chlorine gas buffer tank after the liquid chlorine vaporizes, enters the filter at 180kg / h, and finally passes into the reaction kettle;

[0022] Turn on the tail gas absorption device, keep the reaction kettle under slight negative pressure, react with chlorine gas at 120°C for 40 hours, and add 0.5 kg of catalyst azobisisobutyronitrile per hour. Cooling water was passed through the jacket of the kettle to lower the temperature to 60° C., and the c...

Embodiment 2

[0029] Prepare according to the preparation method of p-chlorobenzoyl chloride in embodiment 2, only change the following parameters of the following steps of embodiment 1:

[0030] 1. Chlorination:

[0031] Add 3400kg p-chlorotoluene, 90kg thionyl chloride and 0.1kg triethanolamine to the reactor and heat up to 85°C;

[0032] Add 0.5kg to the weighing orientation system first, and gradually add the remaining azobisisobutyronitrile during the reaction process;

[0033] The chlorine gas enters the liquid chlorine vaporizer through the liquid phase tube after being measured by the electronic scale of the liquid chlorine cylinder, and is heated by the hot water in the vaporizer. After the liquid chlorine is vaporized, it enters the chlorine gas buffer tank, enters the filter at a certain flow rate of 180kg / h, and finally passes into the reaction kettle;

[0034] Turn on the tail gas absorption device, keep the reaction kettle at a slight negative pressure, react with chlorine ga...

Embodiment 3

[0039] Prepare according to the preparation method of p-chlorobenzoyl chloride in embodiment 3, only change the following parameters of the following steps of embodiment 1:

[0040] 1. Chlorination:

[0041] Add 3400kg p-chlorotoluene, 105kg thionyl chloride and 0.11kg triethanolamine to the reactor and heat up to 85°C;

[0042] Weigh 20kg of azobisisobutyronitrile, add 0.5kg to the system first, and gradually add the remaining azobisisobutyronitrile during the reaction;

[0043] The chlorine gas enters the liquid chlorine vaporizer through the liquid phase tube after being measured by the electronic scale of the liquid chlorine cylinder, and is heated by the hot water in the vaporizer. After the liquid chlorine is vaporized, it enters the chlorine gas buffer tank, enters the filter at a certain flow rate of 180kg / h, and finally passes into the reaction kettle;

[0044] Turn on the tail gas absorption device, keep the reaction kettle under slight negative pressure, react with...

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PUM

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Abstract

The invention discloses a preparation method of parachlorobenzoyl chloride. The method includes the steps of: (1) chlorination: adding the raw material p-chlorotoluene into a reaction kettle, performing stirring, adding triethanolamine into the reaction kettle, and conducting stirring for 30min, adding thionyl chloride, conducting stirring for 10min, then slowing raising the temperature, adding azodiisobutyronitrile, introducing chlorine gas for reaction to obtain 4-chlorobenzotrichloride; (2) hydrolysis: adding the4-chlorobenzotrichloride obtained in step (1) into a hydrolysis kettle, adding the catalyst ferric trichloride, adding water dropwise to obtain a parachlorobenzoyl chloride crude product; and (3) distillation: distilling the parachlorobenzoyl chloride crude product to obtain the product. Specifically, the p-chlorotoluene is 30000-40000 parts, and triethanolamine is 1-10 parts. P-chlorotoluene is adopted as the raw material for chlorination by chlorine gas to obtain 4-chlorobenzotrichloride, and then hydrolysis and distillation are carried out so as to obtain the product. Firstly triethanolamine is utilized to remove the influence of iron ions, then thionyl chloride is utilized to remove the moisture influence, the chlorination reaction time is short, the reaction by-product is few, and the yield is high.

Description

technical field [0001] The invention belongs to a preparation method of p-chlorobenzoyl chloride. Background technique [0002] With the rapid development of polymer materials, p-chlorobenzoyl chloride, as an important chemical intermediate, has attracted more and more attention from researchers. Its excellent performance has been widely used in pharmaceutical intermediates, dye intermediates and preservatives. a wide range of applications. [0003] Existing preparation method is generally to take p-chlorotoluene, chlorine, azobisisobutyronitrile, iron trichloride, water as raw material, through steps such as chlorination, hydrolysis, distillation, produce qualified p-chlorobenzoyl chloride; Discharge at high altitude after washing with water and alkali, and by-product hydrochloric acid and sodium hypochlorite. The shortcoming of this preparation method: 1, the chlorination reaction time is long. 2. There are many side reactions and impurities, and the product yield is lo...

Claims

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Application Information

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IPC IPC(8): C07C63/70C07C51/58C07C25/02C07C17/14
Inventor 于俊田张玲
Owner 山东福尔有限公司
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