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Electron-deficient alkene free radical polymerization method

An electron-deficient and free radical technology, applied in the field of polymer synthesis, can solve the problems of uncontrollable polymer molecular weight, complex preparation process, wide molecular weight distribution, etc., to achieve clear and controllable polymer structure, simple preparation process, and reaction components little effect

Active Publication Date: 2019-03-01
湖南亿明新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem solved by the present invention is that the molecular weight of the polymer obtained by traditional free radical polymerization is uncontrollable, and the molecular weight distribution is relatively wide; traditional living / controllable free radical polymerization needs to be carried out under anhydrous and oxygen-free conditions, and expensive ingredients need to be used. solid and volatile organic solvents, the preparation process is complicated and the cost is high

Method used

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  • Electron-deficient alkene free radical polymerization method
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  • Electron-deficient alkene free radical polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Continuous precipitation polymerization of acrylonitrile in water.

[0032] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), FeCl 3 ·6H 2 O (0.54g, 0.002mol) and 75mlH 2 O, stir and heat up to 60°C; add hydrogen peroxide-water solution 25g (wt.%=3.4%, 0.025mol) dropwise at a rate of d / 1s until the addition is complete, and react for 1h; Suspended solids appeared; the reaction solution was filtered to obtain a crude product, washed three times with deionized water, and dried to obtain 24.94 g of white powder, with a yield of 94.1%. That 1 H-NMR (400MHz, DMSO) spectrum as figure 1 shown.

Embodiment 2

[0033] Example 2: Living / Controlled Free Radical Polymerization of Acrylonitrile in DMF.

[0034] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), FeCl 3 ·6H 2 O (0.54g, 0.002mol) and 75ml of DMF, stirred and heated to 60°C; dropwise added 25g of hydrogen peroxide-DMF solution (wt.% = 3.4%, 0.025mol) at a rate of d / 1s, until the dropwise addition was completed, reflux reaction 2h; the reaction liquid was precipitated by adding water, and the crude product was obtained by filtration, washed three times with deionized water, and dried to obtain 25.76 g of white powder, with a yield of 97.2%.

Embodiment 3

[0035] Example 3: Living / Controlled Free Radical Polymerization of Acrylonitrile in DMSO.

[0036] In a 500ml three-necked flask, add acrylonitrile (26.50g, 0.500mol), 0.27gFeCl 3 ·6H 2 O (0.27g, 0.001mol) and 75ml of DMSO, stirred and heated to 60°C; added dropwise 25g of hydrogen peroxide-DMSO solution (wt.%=4.1%, 0.030mol) at a speed of d / 1s, until the addition was completed, and reacted for 2h Add water to the reaction solution to precipitate, filter to obtain the crude product, wash with deionized water 3 times, and dry to obtain 25.20 g of white powder with a yield of 95.1%.

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Abstract

The invention discloses an electron-deficient alkene free radical polymerization method. The method comprises the steps that an electron-deficient alkene monomer and a chain transfer initiator are dissolved in a reaction solvent, H2O2 is added as an initiator, and free radical polymerization is carried out, wherein the chain transfer initiator is one or a mixture of several of iron chloride, ironbromide, copper chloride and copper bromide. The reaction system only has four components with no other additives required; the reaction components are few, and the application range is wide; residualmetal halide is easy to remove; the polymer structure is clear and controllable; the raw materials are cheap and readily available; reaction can be carried out with water at normal temperature with no severe reaction condition and expensive ligand required; a preparation process is simple, and the production cost is significantly reduced; and side reaction is less, the polymerization is stable and controllable, and therefore, a functional polymer with narrow molecular weight distribution can be obtained more easily.

Description

technical field [0001] The invention relates to a method for free-radical polymerization of electron-deficient olefins, in particular to a new initiation system for free-radical polymerization, which belongs to the technical field of polymer synthesis. Background technique [0002] Free radical polymerization is widely used in the preparation of macromolecular polymers. The polymerization conditions are mild, the monomers are widely applicable, and the operation is simple. It is suitable for almost all polymerization implementation methods. However, due to the reaction characteristics of slow initiation, rapid growth and rapid termination of free radical polymerization, chain termination and chain transfer are prone to occur during the reaction process, which affects the molecular weight and distribution of polymer molecules, making the molecular weight and structure of the polymer Uncontrollable, even cross-linking, branching and other phenomena appear, seriously affecting ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/44C08F120/06C08F120/56C08F2/38
CPCC08F2/38C08F120/06C08F120/44C08F120/56C08F2500/03
Inventor 邓剑如钟隆崔敏刘旭张平安刘思萌李通情
Owner 湖南亿明新材料有限公司