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Purification device and purification method of high-purity isophthaloyl chloride

A technology for isophthaloyl chloride and crude isophthaloyl chloride, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve high production energy consumption, environmental pollution, and difficult distillation methods and other issues, to achieve the effect of high product utilization, good application prospects, and low energy consumption

Active Publication Date: 2016-03-16
宁夏宁东泰和化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the early days, the purification of isophthaloyl dichloride used the recrystallization method. Due to the large amount of solvent used in the purification process, there was an environmental pollution problem, and a large amount of recovered solvent needed to be repurified before being reused, so the production consumed energy. is also relatively high, and this method has basically been eliminated
[0005] Rectification process is a kind of purification method of isophthaloyl dichloride in common use now, adopts the method of rectification purification, can obtain the high-purity isophthaloyl dichloride of more than 99.9%, but for further improving isophthaloyl dichloride product In terms of high quality, maintaining the stability of product quality and reducing costs, there are certain difficulties in the rectification method

Method used

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  • Purification device and purification method of high-purity isophthaloyl chloride

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Experimental program
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Effect test

Embodiment 1

[0028] The purifying device of high-purity isophthaloyl dichloride of the present embodiment comprises the heat exchange tube 2 coiled in the crystallizer body 3, and the crystallizer body 3 is provided with a feeding port 4, a discharge port 9 and a heat exchange tube 2 Connected circulating water inlet 1, circulating water outlet 7, circulating water thermometer 6 is installed on the pipeline of circulating water inlet 1, internal thermometer 10 is installed inside the crystallizer body 3, in order to remove the air in the crystallizer body 3 before feeding, The crystal body 3 is also provided with nitrogen gas and an exhaust port 2 , and the outside of the crystallizer body 3 is provided with an external jacket 8 for heat preservation.

Embodiment 2

[0030] The purification method of the isophthaloyl chloride of the present embodiment may further comprise the steps:

[0031] 1. First, add the melted isophthaloyl chloride synthesis solution into the crystallizer, and raise the temperature to 55°C to ensure that the finished product of the acid chloride is completely melted. The temperature of the reactor was lowered to 45°C and allowed to stabilize for a period of time.

[0032] 2. Then slowly cool down to about 30°C at a rate of 0.002°C / min, let off the low melting point mother liquor, weigh it and carry out content analysis;

[0033] 3. Subsequently, the "sweating" operation is carried out, that is, the temperature in the reactor is gradually increased, and the coarse crystals in the crystal body are partially melted to make the impurities be discharged in the form of "sweat". The sweat is taken at any time during the sweating process for analysis. The temperature rises at a rate of ℃ / min, and the final temperature of sw...

Embodiment 3

[0036] The purification method of the isophthaloyl chloride of the present embodiment may further comprise the steps:

[0037] 1. First, add the melted isophthaloyl chloride synthesis solution into the crystallizer, raise the temperature to 55°C to ensure that the finished product of acid chloride is completely melted, lower the temperature of the reactor to 45°C, and stabilize for a period of time;

[0038] 2. Then slowly cool down to about 35°C at a rate of 0.008°C / min, let off the low melting point mother liquor, weigh it and conduct content analysis;

[0039] 3. Subsequently, the "sweating" operation is carried out, that is, the temperature in the reactor is gradually increased, the coarse crystals in the crystal body are partially melted and the impurities are discharged in the form of "sweat", and the sweat is taken at any time during the sweating process for analysis. The temperature rises at a rate of 1 min, and the final temperature of sweating is 44°C;

[0040] 4. F...

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Abstract

The invention relates to a purification device and a purification method of high-purity isophthaloyl dichloride, and belongs to the technical field of purification of organic matters. The purification device comprises a heat exchange tube which is coiled in a crystallizer body; a feeding port, a discharging port, a circulating water inlet and a circulating water outlet are formed in the crystallizer body; the circulating water inlet and the circulating water outlet are communicated with the heat exchange tube; a circulating water thermometer is arranged on the pipe of the circulating water inlet; an inner thermometer is arranged in the crystallizer body. According to the purification device and the purification method of high-purity isophthaloyl dichloride, the structural design is reasonable, the preparation process is simple, the energy consumption is low, the low-temperature operation can be realized and the product purity can be more than 99.97%.

Description

technical field [0001] The invention relates to a melting crystallization purification device and a purification method of high-purity isophthaloyl dichloride, belonging to the technical field of organic matter purification. Background technique [0002] High-purity isophthaloyl chloride is one of the main raw materials for the production of high-performance meta-aramid fibers, and can also be used as monomers for polyamides, polyesters, polyarylates, polyaramids, and liquid crystal polymers. At the same time, it can also be used as a modifier of high polymers, an intermediate in pesticides and pharmaceutical industries. Therefore, the development of isophthaloyl dichloride products is of great significance, especially the prospect of developing high-purity isophthaloyl dichloride used as a raw material for high-quality meta-aramid fibers is very broad. [0003] At present, the methods for producing isophthaloyl chloride at home and abroad mostly adopt the thionyl chloride ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D9/02C07C51/64C07C63/24
Inventor 黄蒙蒙王超庞帅谢磊辛伟娟朱美宇
Owner 宁夏宁东泰和化学科技有限公司