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A kind of industrial production process for preparing high-purity cyclopentadiene

A technology of cyclopentadiene and production process, which is applied in the chemical industry, distillation purification/separation, sustainable manufacturing/processing, etc., can solve the problems of coking, low level, bumping purity, etc., and achieves improved reaction yield and solution. The effect of complete polymerization and increased reaction temperature

Active Publication Date: 2021-06-04
山东省阳信科瑞实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process solves the problems of coking, bumping and low purity in the existing process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First add diluent 1 (n-dodecane and n-hexane in a mass ratio of 10:3) and polymerization inhibitor 1 (hydroquinone and aniline in a mass ratio of 10:1) into dicyclopentadiene and mix evenly , the amount of diluent 1 is to dilute the raw material to a mass fraction of 20%, and the amount of polymerization inhibitor 1 is 0.01% of the mass of the raw material before dilution. Then carry out depolymerization and rectification separation in the reactive distillation column 1, the temperature of the control column is 190-200°C, the temperature at the top of the tower is 41-45°C, the pressure at the top of the tower is 13-16KPaG, the reflux ratio is 8, and the feed rate Be 3L / min, collect at tower top and obtain thick cyclopentadiene, then thick cyclopentadiene and diluent 2 (n-hexadecane and normal hexane form with 10:3 mass ratio), polymerization inhibitor 2 (2 , 6-di-tert-butyl-p-cresol and tetrachlorobenzoquinone are composed in a mass ratio of 1:1) into the evaporating ke...

Embodiment 2

[0028] First add diluent 1 (n-dodecane and n-hexane in a mass ratio of 15:1) and polymerization inhibitor 1 (hydroquinone and aniline in a mass ratio of 4:1) into dicyclopentadiene and mix well , the amount of diluent 1 is to dilute the raw material to a mass fraction of 20%, and the amount of polymerization inhibitor 1 is 0.01% of the mass of the raw material before dilution. Then carry out depolymerization and rectification separation in the reactive distillation column 1, control the temperature of the tower tank to be 180-190°C, the temperature of the tower top to be 41-43°C, the pressure of the tower top to be 15KPaG, the reflux ratio to be 6, and the feed rate to be 5L / min, collected at the top of the tower to obtain crude cyclopentadiene, then the crude cyclopentadiene and diluent 2 (n-hexadecane and normal hexane are formed in a mass ratio of 5:1), polymerization inhibitor 2 (2,6 -di-tert-butyl-p-cresol and chlorobenzoquinone are composed in a mass ratio of 5:1) into ...

Embodiment 3

[0030] First add diluent 1 (n-dodecane and n-hexane in a mass ratio of 10:1) and polymerization inhibitor 1 (hydroquinone and aniline in a mass ratio of 15:1) into dicyclopentadiene and mix evenly , the amount of diluent 1 is to dilute the raw material to a mass fraction of 25%, and the amount of polymerization inhibitor 1 is 0.01% of the mass of the raw material before dilution. Then carry out depolymerization and rectification separation in the reactive distillation column 1, control the temperature of the tower bottom to be 200°C, the temperature of the tower top to be 41-43°C, the pressure of the tower top to be 13KPaG, the reflux ratio to be 8, and the feed rate to be 1L / min , collect at the top of the tower to obtain crude cyclopentadiene, and then combine crude cyclopentadiene with diluent 2 (n-hexadecane and normal hexane are formed in a mass ratio of 5:1), polymerization inhibitor 2 (2,6-di tert-butyl-p-cresol and chlorobenzoquinone with a mass ratio of 1:5) are added...

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Abstract

The invention provides an industrial production process for preparing high-purity cyclopentadiene by depolymerizing dicyclopentadiene. Dicyclopentadiene is used as a raw material, and diluent 1 and polymerization inhibitor 1 are added to dicyclopentadiene and mixed uniformly, and then Carry out depolymerization and rectification separation in the reactive distillation column 1, collect at the top of the tower to obtain crude cyclopentadiene, then add the crude cyclopentadiene, diluent 2, and polymerization inhibitor 2 into the evaporator, heat and vaporize, and Let the steam pass through a cracking tube for tubular cracking. After cracking, perform secondary depolymerization and rectification separation in the reactive distillation tower 2, and collect high-purity cyclopentadiene at the top of the tower. The process solves the problems of coking, bumping and low purity in the existing process, obtains high-purity cyclopentadiene with a high yield, and has high industrial application value.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to an industrial production process for preparing high-purity cyclopentadiene by depolymerizing dicyclopentadiene. Background technique [0002] Dicyclopentadiene (DCPD for short) is a dimer of cyclopentadiene (CPD). DCPD is a colorless crystal at room temperature. When it contains impurities, it is a light yellow oily liquid with a camphor smell. It has a melting point of 32°C and a boiling point of 170°C. It is soluble in most organic solvents and can be depolymerized into CPD at high temperature. CPD is easily depolymerized at room temperature. Dimerization into DCPD. DCPD mainly comes from the by-products of petroleum cracking, and the yield of C5 fractions using naphtha or light oil as cracking raw materials is relatively high. DCPD has two isomers of bridging ring and hanging ring in the spatial structure. DCPD and its monomer CPD have conjugated double bonds and active hydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/15C07C4/22C07C7/04
CPCC07C4/22C07C7/04C07C2601/10C07C13/15Y02P20/10
Inventor 黄月金孙德兰
Owner 山东省阳信科瑞实业有限公司
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