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Separation method of chloro isoamylene

The technology of a chloroisoamylene and a separation method is applied in the field of vacuum rectification and separation to obtain chloroisoamylene, which can solve the problems of low product purity in the second tower and large return amount in the first tower, etc. The effect of improving distillation yield

Inactive Publication Date: 2007-07-18
上海博爱化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the isomerization of 1-chlorine to 3-chlorine in the rectification process, there is a defect that the return volume of the first tower is large and the purity of the product of the second tower cannot be improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The addition solution (1-chlorine content 70%) is preheated and fed into the middle part of a continuous rectification tower composed of two towers in series. The pressure of the first tower is controlled at -0.092Mpa, the temperature at the top of the tower is controlled at 35°C, and the temperature at the bottom of the tower is 57°C. The reflux ratio is 3, continuous rectification, and the reflux tank divides water regularly to ensure that the reflux components entering the tower do not contain free acid. The output components of the reflux tank return to the first tower after isomerization and water separation; , the pressure of the second tower is controlled at -0.094Mpa, the temperature at the top of the tower is controlled at 39°C, the temperature at the bottom of the tower is 65°C, the reflux ratio is 1, and 98% of the 1-chloro product is obtained by continuous rectification, and the rectification yield is 91%.

Embodiment 2

[0016] The addition liquid (1-chlorine content 70%) is preheated and sent to the middle of a continuous distillation column consisting of two towers in series. The pressure of the first tower is controlled at -0.082Mpa, the temperature at the top of the tower is controlled at 48°C, and the temperature at the bottom of the tower is 67°C. The reflux ratio is 3, continuous rectification, and the reflux tank divides water regularly to ensure that the reflux components entering the tower do not contain free acid. The output components of the reflux tank return to the first tower after isomerization and water separation; , the pressure of the second tower is controlled at -0.092Mpa, the temperature at the top of the tower is controlled at 45°C, the temperature at the bottom of the tower is 70°C, the reflux ratio is 1, and 97.2% of the 1-chloro product is obtained by continuous rectification, and the rectification yield is 91%.

Embodiment 3

[0018] The addition solution (1-chlorine content 70%) is preheated and sent to the middle part of a continuous rectification tower composed of two towers in series. The pressure of the first tower is controlled at -0.095Mpa, the temperature at the top of the tower is controlled at 32°C, and the temperature at the bottom of the tower is 55°C. The reflux ratio is 4, continuous rectification, and the reflux tank divides water regularly to ensure that the reflux components entering the tower do not contain free acid. The output components of the reflux tank return to the first tower after isomerization and water separation; , The pressure of the second tower is controlled at -0.096Mpa, the temperature at the top of the tower is controlled at 38°C, the temperature at the bottom of the tower is 65°C, the reflux ratio is 2, and 97.2% of the 1-chloro product is obtained by continuous rectification, and the rectification yield is 91%.

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Abstract

This invention relates to a separation method of chlor-isoamylene. First preheats the output of isoprene react with hydrogen chloride; then send the output into the first tower central of continuous distillation tower which includes two series towers for vacuum distillation; the first tower pressure is -0.070 ~ - 0.100MPa, the top temperature of 30 ~ 60 deg C, the temperature of the tower reactor is 50 ~ 70 deg C, reflux ratio is 2 ~ 5; reflux pot of first tower has a Layered device for regular separating water; outputs component of reflux pot enter isomerism reactor for isomerism reaction, after water separating return to first tower; tower reactor components enter central of second tower, pressure is - 0.08 ~ 0.10MPa, the top temperature of 30 ~ 50deg, tower reactor temperature of 60 ~ 80 deg C, reflux ratio is 1-3, store the products of consecutive distillation in the tank with cooling jacket. Compared with existing technologies, this invention has energy-saving, high purity features.

Description

technical field [0001] The invention relates to the field of chemical intermediate production and chemical separation technology, in particular to a method for obtaining chlorinated isopentene by vacuum distillation and separation of the addition product of isoprene and hydrogen chloride. Background technique [0002] Chloroisoamylene refers to 1-chloro-3-methyl-butene-2 ​​(referred to as "1-chloro"), which is an important intermediate for the synthesis of pharmaceuticals, spices and pesticides. The product formed by the reaction of isoprene with hydrogen chloride is its mixture with 3-chloro-3-methyl-butene-1 (referred to as "3-chloro"), accompanied by a small amount of series by-product dichloroisopentane . [0003] Generally, the two-tower separation method is adopted, the first tower removes light, the top component returns to isomerization to increase the 1-chlorine content, and then enters the tower for rectification, the tower bottom component enters the second tower...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/04C07C17/383
Inventor 周志刚严国钧张金平郝刚沈强
Owner 上海博爱化工有限公司
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