Method for preparing high-purity cyclopentadiene

A technology for cyclopentadiene and dicyclopentadiene is applied in the field of preparing high-purity cyclopentadiene by a liquid-phase indirect continuous depolymerization method, which can solve the problems of difficult recovery of heat-conducting oil of inert diluent, hindered equipment operation, etc. Low, easy to control, stable product quality

Active Publication Date: 2011-05-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Foreign patent (WO0236529A1) report, SAMAUNG company adopts liquid phase indirect depolymerization method, produces cyclopentadiene, depolymerization temperature 180~210 ℃, depolymerization rate 90%, adopts single polymerization inhibitor, but inert diluent (carrier heat conduction Oil) recovery is more difficult
At present, the liquid-phase indirect thermal depolymerization method mainly has coking or high polymers produced by olefin polymerization are brought into the carrier heat transfer oil, which hinders the long-term operation of the equipment.

Method used

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  • Method for preparing high-purity cyclopentadiene
  • Method for preparing high-purity cyclopentadiene

Examples

Experimental program
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Effect test

Embodiment 1

[0021] First, add pure heat transfer oil and composite polymerization inhibitor with a weight ratio of 1:0.005 to the thermal decomposer 2 and rectification reboiler 6, and then pass in nitrogen to replace the air in the system, heat the heat transfer oil to 270°C, and then pass the metering The pump adds crude dicyclopentadiene (83.5% by mass) from the bottom of the thermal decomposer to the thermal decomposer, contacts with high-temperature heat transfer oil, and controls the feed rate so that it stays in the thermal decomposer for 2.0S, dicyclopentadiene Diene gasification, depolymerized cyclopentadiene enters rectification column 3 for rectification, and the high-purity cyclopentadiene separated from the top of the tower enters collector 5 through condenser 4 (preserved at low temperature), and a small amount of uncracked cyclopentadiene Dicyclopentadiene and by-products are heated in the bottom reboiler 6 and rectified again. The composite inhibitor is a compound of hydro...

Embodiment 2

[0024] First, add pure heat transfer oil and composite polymerization inhibitor with a weight ratio of 1:0.008 to the thermal decomposer 2 and rectification reboiler 6, and then pass in nitrogen to replace the air in the system, heat the heat transfer oil to 280°C, and then pass the metering The pump adds crude dicyclopentadiene (83.5% by mass) from the bottom of the thermal decomposer to the thermal decomposer, contacts with high-temperature heat transfer oil, and controls the feed rate so that it stays in the thermal decomposer for 2.0S, dicyclopentadiene Diene gasification, depolymerized cyclopentadiene enters rectification column 3 for rectification, and the high-purity cyclopentadiene separated from the top of the tower enters collector 5 through condenser 4 (preserved at low temperature), and a small amount of uncracked cyclopentadiene Dicyclopentadiene and by-products are heated in the bottom reboiler 6 and rectified again. The complex polymerization inhibitor is a comp...

Embodiment 3

[0027] First, add pure heat transfer oil and composite polymerization inhibitor with a weight ratio of 1:0.01 to the thermal decomposer 2 and rectification reboiler 6, and then pass in nitrogen to replace the air in the system, heat the heat transfer oil to 280°C, and then pass the metering The pump adds crude dicyclopentadiene (92.7% by mass) from the bottom of the thermal decomposer to the thermal decomposer, contacts with high-temperature heat transfer oil, and controls the feed rate so that it stays in the thermal decomposer for 1.5S. Diene gasification, depolymerized cyclopentadiene enters rectification column 3 for rectification, and the high-purity cyclopentadiene separated from the top of the tower enters collector 5 through condenser 4 (preserved at low temperature), and a small amount of uncracked cyclopentadiene Dicyclopentadiene and by-products are heated in the bottom reboiler 6 and rectified again. The complex polymerization inhibitor is a compound of 4-tert-buty...

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Abstract

The invention relates to a method for preparing high-purity cyclopentadiene, which comprises the following steps of: heating a thermal decomposer containing purified conduction oil and a composite inhibitor and a rectifying reboiler to a specified temperature; adding dicyclopentadiene serving as a crude product into the thermal decomposer continuously and stably; allowing the depolymerized cyclopentadiene to enter a rectifying column; extracting high-purity cyclopentadiene from a tower top, heating a small amount of dicyclopentadiene and by-products by the reboiler at the tower bottom to rectify the small amount of dicyclopentadiene and by-products again, and recycling kettle liquid. The method has the advantages of simple equipment, high production capacity, little coking and long service life of the conduction oil serving as a raw material and the equipment.

Description

Technical field: [0001] The invention relates to a method for preparing high-purity cyclopentadiene, and more specifically relates to a method for preparing high-purity cyclopentadiene by using a liquid-phase indirect continuous depolymerization method using polyester-grade dicyclopentadiene as a raw material. Background technique: [0002] Cyclopentadiene (CPD for short) is an important chemical intermediate with a wide range of uses and is a raw material for the synthesis of pesticides, plastics, and rubber. In recent years, the use of cyclopentadiene to hydrogenate cyclopentene to produce cyclopentene, and then to produce glutaraldehyde, cyclopentanone and other fine chemical products has attracted extensive attention from various countries. [0003] As far as the current technology is concerned, the production of cyclopentadiene mainly adopts the thermal depolymerization method of dicyclopentadiene, which is divided into liquid phase direct or indirect depolymerization m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/15C07C4/22
Inventor 陈万友李正石大川刘宇王龙辉李长途吴辉刘绍岩吴涛杨生
Owner PETROCHINA CO LTD
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