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Method for preparing liquid polyisoprene rubber based on reversible addition-pyrolysis chain transfer radical polymerization and rubber material

A polyisoprene and cracking chain transfer technology, applied in the field of rubber materials, can solve the problems of harsh reaction environment, dangerous storage and use, expensive catalysts, etc., and achieve the effects of less VOC release, easy storage and non-volatile

Pending Publication Date: 2020-07-10
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, anionic polymerization has strict requirements on the reaction environment. As the price of lithium rises, the price of the catalyst is relatively expensive, and the catalyst is highly active, flammable and explosive, and has great dangers in storage and use.

Method used

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  • Method for preparing liquid polyisoprene rubber based on reversible addition-pyrolysis chain transfer radical polymerization and rubber material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of liquid polyisoprene rubber based on RAFT polymerization, specifically:

[0026] Add 45g of 1,4-dioxane, 0.207g of BDAAT, 0.021g of DTBP, and 15g of isoprene into the Erlenmeyer flask in sequence, mix well, transfer the mixture to the reaction kettle, and use liquid nitrogen to The reaction kettle was frozen for 20 minutes, vacuumed with a vacuum pump and nitrogen was reciprocated three times, a pressure of 2 MPa was applied with nitrogen, and the reaction was carried out at 126°C for 10 hours. The product was precipitated with methanol to obtain a yellow liquid product, which was dried in a vacuum oven to constant weight. After calculation, the yield is 19.0%, Mn=0.96×10 4 , Mw / Mn=1.69.

Embodiment 2

[0028] Preparation of liquid polyisoprene rubber based on RAFT polymerization, specifically:

[0029] Add 45g of 1,4-dioxane, 0.5354g of DDMAT, 0.0430g of DTBP, and 15g of isoprene into the Erlenmeyer flask successively, mix well, transfer the mixed solution to the reaction kettle, and use liquid nitrogen to The reaction kettle was frozen for 20 minutes, vacuumed with a vacuum pump and nitrogen was reciprocated three times, a pressure of 2 MPa was applied with nitrogen, and the reaction was carried out at 126°C for 10 hours. The product was precipitated with methanol to obtain a yellow liquid product, which was dried in a vacuum oven to constant weight. After calculation, the yield is 27.0%, Mn=0.49×10 4 , Mw / Mn=1.23.

Embodiment 3

[0031] Preparation of liquid polyisoprene rubber based on RAFT polymerization, specifically:

[0032] Add 45g of 1,4-dioxane, 0.2677g of DDMAT, 0.0215g of DTBP, and 15g of isoprene to the Erlenmeyer flask successively, mix well, transfer the mixed solution to the reaction kettle, and use liquid nitrogen to The reaction kettle was frozen for 20 minutes, evacuated by a vacuum pump to pass nitrogen gas back and forth three times, and a pressure of 2 MPa was applied with nitrogen gas, and reacted at 126°C for 10 hours. The product was precipitated with methanol to obtain a yellow liquid product, which was dried in a vacuum oven to constant weight. After calculation, the yield is 21.6%, Mn=0.7×10 4 , Mw / Mn=1.32.

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Abstract

The invention provides a method for preparing liquid polyisoprene rubber based on reversible addition-pyrolysis chain transfer radical polymerization. The preparation method comprises the following steps: uniformly mixing isoprene, an RAFT reagent, a solvent and an initiator and then putting a mixture into a reaction device, carrying out freezing pumping drainage on the reaction device by using liquid nitrogen, applying pressure by using nitrogen or inert gas, and carrying out polymerization reaction for 10-30 hours at the reaction pressure of 0.1-4Mpa and the reaction temperature of 80-130 DEG C to obtain the liquid polyisoprene rubber. The molecular weight distribution of the obtained liquid polyisoprene rubber is 1.2-2.0, the number-average molecular weight is 0.5*10<4> to 2.5*10<4>, and the liquid polyisoprene rubber can be added into a rubber matrix to be used as a reactive plasticizer. Compared with traditional plasticizers such as aromatic hydrocarbon oil, the liquid isoprene rubber has the advantages of being good in plasticizing effect, free of migration and extraction by a solvent, not prone to volatilization at high temperature, less in VOC release and the like.

Description

technical field [0001] The invention relates to the field of chemically synthesized rubber, in particular to a method and rubber material for preparing liquid polyisoprene rubber based on reversible addition-cracking chain transfer radical polymerization. Background technique [0002] Due to the high Mooney viscosity, the mixing process of rubber usually requires the use of additives to reduce the viscosity so that it has a certain fluidity at a certain temperature. Liquid oils such as aromatic oil, TDAE, naphthenic oil, paraffin oil, etc. are the most commonly used plasticizers in the rubber industry, and most of them are polycyclic aromatic compounds, which are polluting and harmful to the human body; The quality is low, the heat resistance is poor, it is easy to extract or migrate in the rubber compound, and it is easy to volatilize at high temperature, resulting in more VOC release, which limits its application in multi-phase composite systems. The EU REACH regulations ...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F2/38
CPCC08F136/08C08F2438/03C08F2/38
Inventor 王润国辛明泽张立群陈加平迟乐
Owner BEIJING UNIV OF CHEM TECH
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