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A method for directly preparing epoxidized conjugated diene polymer with conjugated diene solution polymerization stock solution

A technology for epoxidizing conjugated diolefins and conjugated diolefins, which is applied in the field of polymer manufacturing and modification, can solve the problems of difficult recycling and reuse, difficult post-processing of reaction products, and high prices, so as to reduce energy consumption and achieve good Effects of Industrialization Prospects

Active Publication Date: 2020-07-14
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These acidic peroxides are not only expensive as oxygen sources, but also produce acids that are highly corrosive to equipment during the reaction process, making post-processing of the reaction products difficult; and side reactions such as ring opening of epoxy bonds are prone to occur
Literature ("Advances in Organometallic Chemistry", 2015,64:1-39; "Reactive&Functional Polymers", 2005,64(2):83-91) has also reported that using hydrogen peroxide as an oxygen source, in the homogeneous catalyst Partial C=C double bonds in the conjugated diene polymer are epoxidized under the action of catalysts, but this type of catalyst is expensive and difficult to recycle and reuse

Method used

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  • A method for directly preparing epoxidized conjugated diene polymer with conjugated diene solution polymerization stock solution
  • A method for directly preparing epoxidized conjugated diene polymer with conjugated diene solution polymerization stock solution
  • A method for directly preparing epoxidized conjugated diene polymer with conjugated diene solution polymerization stock solution

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get 1,3-butadiene solution polymerization stock solution (brand is the butadiene rubber stock solution of BR 9000, wherein solvent is No. 6 solvent naphtha, butadiene rubber content=29.4wt%) 13.6g, add by 45.6mL normal hexane and 40mL1 , a mixed solvent composed of 2-dichloroethane, dilute the rubber concentration to 40g / L; raise the temperature to 60°C. Simultaneously, 0.20g catalyst (catalyst is the compound that hexadecylpyridinium cation and phosphotungstic acid anion forms, molecular formula is [π-C 5 h 5 NC 16 h 33 ] 3 [PW 4 o 16 ]) and 800μL of 30wt% hydrogen peroxide and 20mL of 1,2-dichloroethane were mixed at 60°C, and slowly added dropwise to the rubber solution, and reacted at 60°C for 2 hours. Wherein the hydrogen peroxide consumption is 10 mol% of the butadiene structural unit in the butadiene rubber, and the catalyst consumption is 5 wt% of the butadiene rubber mass. After the reaction, cool the reaction liquid at 5°C for 15 minutes, wash the solid...

Embodiment 2

[0033] Get 1,3-butadiene solution polymerization stock solution (brand is the butadiene rubber stock solution of BR 9000, wherein solvent is No. 6 solvent naphtha, butadiene rubber content=29.4wt%) 13.6g, add by 45.6mL normal hexane and 40mL1 , a mixed solvent composed of 2-dichloroethane, dilute the rubber concentration to 40g / L; raise the temperature to 60°C. At the same time, mix 0.04g of catalyst, 160μL of 30wt% hydrogen peroxide and 20mL of 1,2-dichloroethane at 60°C, and slowly drop them into the rubber solution, and react at 60°C for 2 hours. Wherein the amount of hydrogen peroxide is 2 mol% of the butadiene structural unit in the butadiene rubber, and the amount of the catalyst is 1 wt% of the mass of the butadiene rubber. After the reaction, cool the reaction liquid at 5°C for 15 minutes, wash the solid matter with a small amount of 1,2-dichloroethane several times after centrifugation, and merge the eluate into the liquid. The solid matter can be directly used for th...

Embodiment 3

[0035] Get 1,3-butadiene solution polymerization stoste (brand is butadiene rubber stoste of BR 9000, wherein solvent is No. 6 solvent naphtha, butadiene rubber content=29.4wt%) 13.6g, add by 45.6mL n-hexane and 40mL Mixed solvent composed of 1,2-dichloroethane, dilute the rubber concentration to 40g / L; heat up to 60°C. At the same time, mix 0.20g of catalyst, 1600μL of 30wt% hydrogen peroxide and 20mL of 1,2-dichloroethane at 60°C, and slowly drop them into the rubber solution, and react at 60°C for 2 hours. Wherein the amount of hydrogen peroxide is 20 mol% of the butadiene structural unit in the butadiene rubber, and the amount of the catalyst is 5 wt% of the mass of the butadiene rubber. After the reaction, cool the reaction liquid at 5°C for 15 minutes, wash the solid matter with a small amount of 1,2-dichloroethane several times after centrifugation, and merge the eluate into the liquid. The solid matter can be directly used for the next time after vacuum drying. Cataly...

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Abstract

The invention discloses a method for directly preparing an epoxidized conjugated diene polymer from polymerization dope of a conjugated diene solution, and belongs to the technical field of polymer production and modification. A polymer dope formed from conjugated diene by solution homopolymerization or copolymerization in a polymerization reactor is taken as a raw material, a hydrogen peroxide solution is used for epoxidizing part of double bonds in the conjugated diene polymer under catalysis of quaternary ammonium phosphotungstate, and an epoxidized conjugated diene homopolymer or copolymeris prepared. In the reaction process, the conversion rate of hydrogen peroxide in the hydrogen peroxide solution can reach 100%, the epoxidizing rate of carbon-carbon double-bonds in the conjugated diene polymer is adjustable in the range of 0.01mol%-50mol%, a catalyst is recovered, and after three times of recycling, the catalytic efficiency of the catalyst can still reach 90% or higher of thatof a fresh catalyst. Compared with use of solid conjugated diene polymer raw materials, solvent removal and drying and polymer breaking and dissolution during preparation are omitted, so that energy consumption can be reduced remarkably, and production efficiency and economic efficiency can be improved.

Description

technical field [0001] The invention belongs to the field of polymer manufacture and modification, and in particular relates to a method for preparing epoxidized conjugated diene polymer by directly using conjugated diene solution polymerization stock solution as raw material. Background technique [0002] Conjugated dienes mainly include 1,3-butadiene and isoprene, and high molecular weight conjugated diene polymers, such as butadiene rubber, can be prepared by solution homopolymerization or solution copolymerization with other vinyl monomers , rare earth butadiene rubber, isoprene rubber, low cis polybutadiene rubber, solution polystyrene butadiene rubber, SBS, SIS thermoplastic elastomer, K resin, etc. Due to the easy availability of raw materials and unique performance, it is widely used in automobiles, ships, rail transit, aerospace vehicles, insulating materials, conveyor belts, shoe materials, etc. However, this kind of conjugated diene polymer does not contain polar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/08C08F36/04
CPCC08F8/08C08F36/04
Inventor 李伯耿徐力介素云范宏吴林波王文俊卜志杨
Owner ZHEJIANG UNIV
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