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A kind of method for continuously preparing 4-chloro-1-butanol

A continuous method and butanol technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as increasing production costs, achieve less waste generation, reduce hazardous waste emissions, and improve dispersion Effect

Active Publication Date: 2022-04-22
常州新东化工发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a large amount of hydrogen chloride by-products in the chlorination process, and it is easy to entrain a small amount of organic matter when the by-product acid is used, and the organic matter needs to be treated to less than 50ppm before it can be sold as a product, thus greatly increasing the production cost

Method used

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  • A kind of method for continuously preparing 4-chloro-1-butanol

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Experimental program
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Effect test

Embodiment 1

[0024] The inner diameter of the intensified reactor is A 2.0m-long pipe reactor with extracorporeal pumping and circulation, and the internal packing is stainless steel θ packing; the preparation process of 4-chloro-1-butanol is as follows:

[0025] 1) THF is added into the enhanced reactor and preheated to 65°C;

[0026] 2) Raise the temperature of the intensified reactor to 95°C, then slowly feed the amount of hydrogen chloride into the reactor according to the molar ratio of tetrahydrofuran to hydrogen chloride of 1:0.31, and control the pressure of the reactor to 1.2MPa, and force a circular reaction. During the reaction, every 0.5h sampling analysis, stop the reaction when the THF conversion rate reaches 30%;

[0027] 3) Add the reaction solution obtained in step 2) to the first rectification tower, control the temperature of the first rectification tower tower bottom to be 35° C., and the pressure of the first rectification tower to be-0.067Mpa, and obtain hydrogen ch...

Embodiment 2

[0030] The difference between this embodiment and Example 1 is that, in step 3), the tetrahydrofuran fraction obtained at the top of the tower is mainly recycled to step (1) for reuse, and 75% of the raffinate in the second rectifying column is recycled to step ( 2) reuse, after the above-mentioned circular reaction is carried out once, 4-chloro-1-butanol is finally obtained at the top of the second rectifying tower, with a yield of 94% and a purity of 99.6%.

Embodiment 3

[0032] The difference between this example and Example 2 is that in step 2), the temperature of the enhanced reactor is raised to 98.5°C, and hydrogen chloride is fed into the enhanced reactor with a molar ratio of tetrahydrofuran to hydrogen chloride of 1:0.62 for forced circulation reaction and the reactor The pressure is 1.25MPa. During the reaction process, the sample is analyzed every 0.5h, and the reaction is stopped when the THF conversion rate reaches 60%. In step 3), the temperature in the bottom of the first rectification tower is 33.6°C, and the rectification pressure is -0.075MPa; In step 4), the temperature at the bottom of the second rectification tower is 70.8°C, and the rectification pressure is -0.098Mpa, and finally 4-chloro-1-butanol is obtained at the top of the second rectification tower with a yield of 95%. Its purity is 99.8%.

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Abstract

The invention discloses a method for continuously preparing 4-chloro-1-butanol. The crude product is obtained by forcibly circulating tetrahydrofuran and hydrogen chloride in a reinforced pipeline reactor equipped with iron fillers, and 4-chloro-1-butanol is obtained through two vacuum distillations. Chlorine-1-butanol, tetrahydrofuran mainly obtained at the top of the first rectifying tower and 70-90% of the residual night of the second rectifying tower still can be recycled. The technological method provided by the invention has high material utilization rate, less waste generation, high product purity, easy control of the reaction process and continuous production.

Description

Technical field: [0001] The invention relates to a preparation method for preparing 4-chloro-1-butanol, more specifically, to a method for preparing 4-chloro-1-butanol by using tetrahydrofuran and hydrogen chloride as raw materials. Background technique: [0002] 4-Chloro-1-butanol is an important fine chemical product, which can be used to synthesize various pesticides and pharmaceutical intermediates, and has wide application prospects. There are a large amount of hydrogen chloride by-products in the chlorination process, and a small amount of organic matter is easily entrained when the by-product acid is used, and the organic matter needs to be treated to below 50ppm before it can be sold as a product, thus greatly increasing the production cost. If the by-product acid is used as a raw material for the production of 4-chloro-1-butanol and comprehensively utilized, it can not only turn waste into treasure, but also improve the economy of the process and embody the concept ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/64C07C29/80C07C31/36
CPCC07C29/64C07C29/80C07C31/36Y02P20/584
Inventor 董亮陶文平马凯王顺利年立春孙运林张驰吴发明郝祥忠张明张鹏陶春平
Owner 常州新东化工发展有限公司
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