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A method for separating bridged tetrahydrocyclopentadiene isomerization products

A technology for hanging tetrahydrodicyclopentadiene and tetrahydrocyclopentadiene is applied in the field of separating bridge-type tetrahydrocyclopentadiene isomerization products, which can solve the problems of difficulty in separating trans-decalin and the like, and achieves the The rectification operation is easy to control, the condensation reaction is avoided, and the method is simple and easy to implement.

Active Publication Date: 2019-07-09
军事科学院系统工程研究院军事新能源技术研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although vacuum distillation can reduce the gasification temperature, it is difficult to separate trans-decalin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for separating bridged tetrahydrocyclopentadiene isomerization products, which sequentially separates the reaction solvent with a boiling point lower than that of hanging tetrahydrodicyclopentadiene, light by-products and hanging tetrahydrodicyclopentadiene. Described light by-product comprises trans-decalin; Concrete steps are as follows:

[0024] (1) Adopt steam rectification to separate the reaction solvent whose boiling point is lower than hanging type tetrahydrocyclopentadiene: put the bridging tetrahydrocyclopentadiene isomerization product in a distillation tower, adopt steam rectification to separate, water The dosage is 0.1-1 times of the reaction solvent in the mixture to be separated, the number of theoretical plates is 10-30, the rectification pressure is 101KPa, the reflux ratio is 0.1:1—1:1, the temperature at the top of the tower is 68-71°C, and the temperature at the bottom of the tower is 81-85°C, the production liquid at the top of the tower i...

Embodiment 2

[0028] Preferably, a method for separating bridged tetrahydrocyclopentadiene isomerization products, sequentially separating the reaction solvent with a boiling point lower than that of hanging tetrahydrodicyclopentadiene, light by-products and hanging tetrahydrodicyclopentadiene Alkene, described light by-product comprises trans-decalin; Concrete steps are as follows:

[0029] (1) Adopt steam rectification to separate the reaction solvent whose boiling point is lower than hanging tetrahydrocyclopentadiene: put the bridged tetrahydrocyclopentadiene isomerization product in a distillation tower, adopt steam rectification to separate, water The dosage is 0.2-0.8 times of the reaction solvent in the mixture to be separated, the number of theoretical plates is 15-25, the rectification pressure is 101KPa, the reflux ratio is 0.1:1—1:1, the temperature at the top of the tower is 68-71°C, and the temperature at the bottom of the tower is 81-85°C, the production liquid at the top of the...

Embodiment 3

[0033] Take 1800 g of bridged tetrahydrodicyclopentadiene isomerization reaction product, which contains about 1200 g of reaction solvent cyclohexane and 600 g of deionized water. Atmospheric pressure steam rectification on a rectification column with a theoretical plate number of 20, the reflux ratio is controlled at 0.3:1, the temperature at the top of the tower is 68-70°C, and the temperature at the bottom of the tower is 81-83°C. After the rectification, the top production liquid is divided into water to obtain about 1180g cyclohexane, and the content of heavier components such as hanging tetrahydrodicyclopentadiene is less than 0.1% according to chromatographic analysis, while the cyclohexane in the remaining organic materials in the tower still The content is less than 0.01%.

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PUM

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Abstract

The invention discloses a method for separating an endo-tetrahydrocyclopentadiene isomerization product, which aims at purifying exo-tetrahydrodicyclopentadiene. The method comprises the following steps of firstly, separating a reaction solvent and a light-weight byproduct by water vapor distillation and multi-element azeotropic distillation, wherein the boiling point of the reaction solvent is lower than the boiling point of the exo-tetrahydrodicyclopentadiene; separating the exo-tetrahydrodicyclopentadiene by water vapor distillation, and separating water from a tower top product of the later, so as to obtain the exo-tetrahydrodicyclopentadiene meeting purity requirement. The technology method has the characteristics that the separation accuracy is high, and an entrainer can be recycled.

Description

technical field [0001] The invention relates to a method for separating bridged tetrahydrocyclopentadiene isomerization products, which belongs to the field of separation engineering of petrochemical industry. Background technique [0002] The hydrogenation product of dicyclopentadiene (DCPD)—bridged tetrahydrodicyclopentadiene can be obtained through isomerization reaction to obtain pendant tetrahydrodicyclopentadiene (exo-THDCPD), which is a low-temperature liquid with excellent performance. Density fuel widely used as propellant for missiles, aircraft and torpedoes. [0003] Molecular sieves are used as bridged tetrahydrodicyclopentadiene isomerization catalysts, although compared with the traditional L strong acid AlCl 3 It has the advantages of being reusable and reducing environmental pollution. However, due to the low surface acid density, a high reaction temperature is required, and other side reactions are prone to occur, resulting in a large amount of by-products ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/06C07C13/61C07C13/50C07C13/615
CPCC07C7/005C07C7/06C07C13/50C07C13/61C07C13/615
Inventor 安高军熊春华赵会吉鲁长波刘晨光周友杰王旭东任连岭
Owner 军事科学院系统工程研究院军事新能源技术研究所
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