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Preparation method of PDCPD raw material containing cyclopentadiene tripolymer

A technology of cyclopentadiene and dicyclopentadiene is applied in the field of preparation of PDCPD raw materials, can solve the problems of low reaction yield, high production cost, reduced yield and the like, achieves simple and reliable process route, reduced side reactions, Reduce the effect of explosion

Pending Publication Date: 2022-06-24
HENGHE MATERIALS & SCI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses an ionic liquid catalyst, and neutralizes and washes with sodium hydroxide, which will cause a large amount of waste water. The claim also mentions decolorization with activated carbon, which will generate a large amount of solid waste, both waste water and solid waste. Waste, very not environmentally friendly
[0008] CN100594204C discloses a synthetic method of cyclopentadiene trimer, in order to solve the problem that the reaction yield is not high
In this method, a solvent is added as a diluent, and then the trimer is separated and concentrated through a rectification tower, which will cause a problem of high production costs.
At the same time, when the distillation tower is separated, the temperature at the bottom of the tower is high, and excessive polymers such as residual oil will be formed, resulting in waste of materials and a decrease in yield.

Method used

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  • Preparation method of PDCPD raw material containing cyclopentadiene tripolymer
  • Preparation method of PDCPD raw material containing cyclopentadiene tripolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] After the dicyclopentadiene feedstock F1 is preheated to 100°C by the feed heater E1, it is mixed with the cyclopentadiene feedstock F3 from the depolymerization unit at a mass ratio of 3:0.5 in the mixer X2. The mixed material is mixed with the pressurized material from the circulating pump P1. The mixing ratio is fresh feed: the mass ratio of circulating material is 1:20. The mixed material enters the polymerization reactor R1, while the second strand of cyclopentadiene is mixed. Material F3 (with a mass ratio of DCPD of 3:0.5) is injected at the stirring paddle of the polymerization reactor R1, and the polymerization reaction is carried out in the polymerization reactor R1. The device E3 controls the hot water F4 fed into the stirred tank R1 at 150°C, the polymerization residence time is controlled by the feed flow to 10h, and the reactor pressure is controlled by the control valve to be 0.5Mpa. Material F5 is produced from the top of the polymerization kettle throug...

Embodiment 2

[0051] After the dicyclopentadiene raw material F1 is preheated to 100 ℃ by the feed heater E1, it is mixed with the antioxidant F2 in the mixer X1. The amount of the antioxidant added is 300ppm of the total fresh feed. The incoming cyclopentadiene material F3 is mixed in the mixer X2 in a mass ratio of 3:0.5. The mixed material is mixed with the pressurized material from the circulating pump P1. The mixing ratio is fresh feed: the mass ratio of circulating material is 1:20. The mixed material enters the polymerization reactor R1, while the second strand of cyclopentadiene is mixed. The material (with a mass ratio of DCPD of 3:0.5) was injected at the stirring paddle of the polymerization reactor R1, and the polymerization reaction was carried out in the polymerization reactor R1. At the same time, the polymerization stirring speed was set to 98r / min, and the polymerization reaction temperature was controlled by the hot water system. At 150°C, the polymerization residence time...

Embodiment 3

[0055] After the dicyclopentadiene raw material F1 is preheated to 100 ℃ by the feed heater E1, it is mixed with the antioxidant F2 in the mixer X1. The amount of the antioxidant added is 300ppm of the total fresh feed. The incoming cyclopentadiene material F3 is mixed in the mixer X2 in a mass ratio of 3:0.5. The mixed material is mixed with the pressurized material from the circulating pump P1. The mixing ratio is fresh feed: the mass ratio of circulating material is 1:20. The mixed material enters the polymerization reactor R1, while the second strand of cyclopentadiene is mixed. The material (with a mass ratio of DCPD of 3:0.5) was injected at the stirring paddle of the polymerization reactor R1, and the polymerization reaction was carried out in the polymerization reactor R1. At the same time, the polymerization stirring speed was set to 98r / min, and the polymerization reaction temperature was controlled by the hot water system. At 160°C, the polymerization residence time...

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Abstract

The invention relates to a preparation method of a PDCPD (dicyclopentadiene) raw material containing a cyclopentadiene tripolymer, which is characterized in that the occurrence of side reactions of multimers such as a dimer and a tetramer is reduced through segmented injection of cyclopentadiene, preheating of DCPD (dicyclopentadiene), adoption of a stirring kettle as a polymerization reactor and precise temperature control, and the preparation method is simple and reliable in process route, low in equipment requirement and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of preparation of dicyclopentadiene, and particularly relates to a preparation method of a PDCPD raw material containing a cyclopentadiene trimer. Background technique [0002] Dicyclopentadiene (DCPD) is the raw material for the synthesis of thermosetting cross-linked polymer polydicyclopentadiene (PDCPD). PDCPD engineering materials have superior impact resistance and stability, and can be used in many engineering fields. The only way to prepare PDCPD is to use reaction injection molding, which requires that the polymerization raw material must be liquid, with very good fluidity and low viscosity. However, the high-purity DCPD raw material has a melting point of 34°C and exists as a solid at room temperature, which brings inconvenience to the use process. By including a certain amount of cyclopentadiene trimer in DCPD, the problem of crystallization of high-purity dicyclopentadiene at room temperature can be avoide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C2/50C07C13/64
CPCC07C2/50C07C2603/91C07C13/64
Inventor 杨孟君李来福孙向东贾立朋
Owner HENGHE MATERIALS & SCI TECH CO LTD
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