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Synthesis method of cyclopentadiene trimer

A technology of cyclopentadiene trimer and dicyclopentadiene, which is applied in the field of preparation of cyclopentadiene trimer, can solve the problems of catalyst solid waste treatment cost, increased catalyst usage, and high equipment requirements, and achieves the realization of The effect of recycling, simplifying the synthesis process, and reducing the requirements of the reaction equipment

Inactive Publication Date: 2019-06-11
广东新华粤石化集团股份公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of the synthesis processes of cyclopentadiene trimer have high temperature and pressure, high requirements on equipment, many side reactions, and low product yield; some increase the use of catalysts, forming catalyst solid waste and high treatment costs

Method used

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  • Synthesis method of cyclopentadiene trimer
  • Synthesis method of cyclopentadiene trimer
  • Synthesis method of cyclopentadiene trimer

Examples

Experimental program
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Effect test

Embodiment 1-6

[0019] Add 1000g of dicyclopentadiene (DCPD) into the batching tank 8 through the reaction feed pipe 1, then add 0.1g of antioxidant BHT through the antioxidant injection line 9, and mix the ethylbenzene according to the ratio of Table 1. uniform. Reactor 7 was repeatedly flushed with nitrogen for replacement until the oxygen content was controlled at 0.1%. Keep the pressure of the reaction kettle 7 at a slight positive pressure, use the metering pump to inject the configured reaction material into the reaction kettle 7 through the reaction material feed pipe 1, and when all the materials are injected, gradually heat the reaction kettle 7, within 2 hours The reaction kettle 7 temperature was raised to the setting temperature in Table 1. Then keep the temperature according to the reaction time in Table 1, stop heating after the completion of the constant temperature. Use a metering pump to pump the material in the reaction kettle 7 through the discharge pipe 6 to the rectific...

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Abstract

The invention discloses a preparation method of cyclopentadiene trimer. The preparation method comprises the following steps: adding an antioxidant into dicyclopentadiene, wherein the mass concentration of the antioxidant is 100-150 ppm; repeatedly feeding nitrogen into a reaction kettle for carrying out replacing on the reaction kettle until the oxygen content in the reaction kettle is controlledto be 0.2% or below; then adding the dicyclopentadiene solution and an inert solvent into the reaction kettle, wherein the mass ratio of the inert solvent to the dicyclopentadiene is 3:7 or 2:8; carrying out a reaction for 20-24 hours at a reaction temperature of 140-180 DEG C and under absolute pressure of 140-180 KPa; then carrying out distillation separation on the reacted mixture in a rectifying tower; and carrying out side-stream extraction to obtain the cyclopentadiene trimer. The preparation method disclosed by the invention only needs to be carried out under a relatively low-temperature and low-pressure reaction condition, so that cost is saved, and purity of the cyclopentadiene trimer obtained by rectification reaches 95% or above.

Description

technical field [0001] The invention relates to a preparation method of cyclopentadiene trimer, which belongs to the technical field of organic synthesis. Background technique [0002] Cyclopentadiene trimer is an important fine chemical intermediate. After hydrogenation, cyclopentadiene trimer can be used to prepare tetrahydrotricyclopentadiene, which can be used as high-density fuel. At present, cyclopentadiene Diene trimers are mainly used as synthetic raw materials for engineering plastics (PDCPD). [0003] The synthesis method of cyclopentadiene trimer is mostly synthesized by the Diels-Alder reaction of dicyclopentadiene and cyclopentadiene. Dicyclopentadiene is decomposed into cyclopentadiene at a certain temperature, and cyclopentadiene is then combined with bicyclopentadiene Pentadiene reacts to form cyclopentadiene trimer. In the known synthesis method of cyclopentadiene trimer, the reaction is mostly carried out under the conditions of high temperature and high ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/64C07C2/50C07C7/04
Inventor 刘阳左洪亮梁国强杨圣儒陈炳琳谭庆梁池辉黄杰
Owner 广东新华粤石化集团股份公司