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Method for separating cyclohexene and 1,3-cyclohexadiene by azeotropic distillation

A technology of cyclohexadiene and azeotropic distillation, which is applied in the direction of distillation purification/separation, chemical instruments and methods, fractional condensation purification/separation, etc., can solve problems such as difficult separation, reduce pollution, reduce operating costs, and save Effect of entrainer recovery tower and product recovery tower

Active Publication Date: 2018-05-29
CHINA TIANCHEN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it contains impurity 1,3-cyclohexadiene, and cyclohexene and 1,3-cyclohexadiene belong to a near-boiling mixture, the boiling point of cyclohexene is 82.9°C, and the boiling point of 1,3-cyclohexadiene is 80.3°C , at the same time, the polarity of the two is similar, so it is difficult to separate and obtain high-purity cyclohexene products by ordinary rectification

Method used

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  • Method for separating cyclohexene and 1,3-cyclohexadiene by azeotropic distillation

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Comparison scheme
Effect test

Embodiment 1

[0026] The technological process of separating cyclohexene and 1,3-cyclohexadiene by azeotropic distillation is as follows: figure 1 shown. The azeotropic distillation column 1 has 40 theoretical plates. Water is used as an entrainer, and it is added from the 15th theoretical plate (the number of plates is from top to bottom), and the addition amount is 150kg / hr. 25 plates were added, the total flow rate was 1500kg / hr, and the mass fraction of cyclohexene was 86wt%. The operating pressure of azeotropic distillation tower 1 is 0kPaG, the reflux ratio at the top of the tower is 0.1, the temperature at the top of the tower is 70.7°C, and the temperature at the bottom of the tower is 95.9°C. The cyclohexene with a mass fraction of 90.7wt% is obtained at the top of the tower, and is decanted at the top of the tower The cyclohexene with a mass fraction of 99.5 wt% is obtained after the decanter 3, and the operating temperature of the overhead decanter 3 is 40° C., and the operatin...

Embodiment 2

[0028] The azeotropic distillation column 1 has 40 theoretical plates. Use water as the entrainer, add from the 15th theoretical plate (the number of plates is from top to bottom), the addition amount is 200kg / hr, cyclohexene and 1,3-cyclohexadiene are added from the 25th plate in the middle of the tower Adding, the total flow rate is 1500kg / hr, wherein the mass fraction of cyclohexene is 86wt%. The operating pressure of azeotropic distillation tower 1 is 0kPaG, the reflux ratio at the top of the tower is 0.1, the temperature at the top of the tower is 70.7°C, and the temperature at the bottom of the tower is 96.3°C. The cyclohexene with a mass fraction of 90.7wt% is obtained at the top of the tower, and is decanted at the top of the tower After the decanter 3, cyclohexene with a mass fraction of 99.8 wt% is obtained, and the operating temperature of the overhead decanter 3 is 40° C., and the operating pressure is 0 kPaG. The 1,3-cyclohexadiene and water mixture at the bottom...

Embodiment 3

[0030] The azeotropic distillation column 1 has 40 theoretical plates. Use water as the entrainer, add from the 15th theoretical plate (the number of plates is from top to bottom), the addition amount is 200kg / hr, cyclohexene and 1,3-cyclohexadiene are added from the 25th plate in the middle of the tower Adding, the total flow rate is 1500kg / hr, wherein the mass fraction of cyclohexene is 86wt%. The operating pressure of azeotropic rectification tower 1 is 10kPaG, the reflux ratio at the top of the tower is 0.1, the temperature at the top of the tower is 72.3°C, and the temperature at the bottom of the tower is 98.5°C. The cyclohexene with a mass fraction of 91.3wt% is obtained at the top of the tower, which is decanted at the top of the tower After the decanter 3, cyclohexene with a mass fraction of 99.7wt% was obtained, and the operating temperature of the overhead decanter 3 was 40° C., and the operating pressure was 10 kPaG. The 1,3-cyclohexadiene and water mixture at the...

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Abstract

The invention provides a method for separating cyclohexene and 1,3-cyclohexadiene by azeotropic distillation. A mixed solution of cyclohexene and 1,3-cyclohexadiene is introduced into an azeotropic distillation tower from the middle of the azeotropic distillation tower, an azeotrope former is also introduced into the azeotropic distillation tower from the middle of the azeotropic distillation tower, overhead gas is condensed by a condenser and enters a tower top decanter for phase splitting and layering, one part of an aqueous phase I flows back to the azeotropic distillation tower through a reflux pump, and the other part serving as a circulating impurity is discharged out of a boundary region; an oil phase I serving as a cyclohexene product is extracted by a cyclohexene product pump; a 1,3-cyclohexadiene and azeotrope former mixture at the tower bottom enters a tower bottom decanter for phase splitting and layering, and an aqueous phase II returns to the azeotropic distillation towerfor recycling by an azeotrope former circulating pump; an oil phase II serving as a 1,3-cyclohexadiene product is extracted by a 1,3-cyclohexadiene product pump, wherein the azeotrope former is water. High-purity cyclohexene and 1,3-cyclohexadiene products can be obtained with the method, utilization rate of by-product heavy oil is increased, operation cost of a device is reduced, and environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the technical field of material separation, in particular to a method for separating cyclohexene and 1,3-cyclohexadiene through azeotropic distillation. Background technique [0002] Cyclohexene is a widely used raw material for organic synthesis, such as synthesizing lysine, cyclohexanone, phenol, polycycloolefin resin, chlorocyclohexane, rubber additives, cyclohexanol raw materials, etc., and can also be used Used as catalyst solvent, petroleum extractant and high octane gasoline stabilizer. Cyclohexene is the main raw material for preparing cyclohexanol and cyclohexanone by hydration method, while cyclohexanol and cyclohexanone are the main raw materials for producing adipic acid and caprolactam respectively. [0003] In the process of preparing cyclohexanol and cyclohexanone by cyclohexene hydration method, various side reactions will occur, resulting in various impurities in the crude alcohol and ketone, and while the pro...

Claims

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Application Information

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IPC IPC(8): C07C7/00C07C7/06C07C7/09C07C13/20C07C13/23
CPCC07C7/005C07C7/06C07C7/09C07C13/20C07C13/23
Inventor 柴永峰李发源李广忠刘新伟李岩李碧柳
Owner CHINA TIANCHEN ENG
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