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Method for preparing high molecular compound adopting novel ion liquid polymerization initiation system

A polymer compound and ionic liquid technology, which is applied in the field of preparing polymer compounds with a new type of ionic liquid polymerization initiation system, can solve the problems of difficult recycling of catalysts, large amount of catalysts, and high processing costs, and achieve a wide range of catalyst selection and avoid toxicity. Influence and avoid the effect of pollution

Inactive Publication Date: 2006-07-26
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are still defects in the current ATRP system: because the polymerization rate is related to the amount of catalyst and ligand, in order to achieve a suitable polymerization rate, the amount of catalyst in the polymerization system is relatively large (1:100); the C-Cl of the initiator in the catalyst system The bond strength is greater than the C-Br bond, so for the Cl-ATRP system, the polymerization temperature is generally 100-130°C; for the Br-ATRP system, the polymerization temperature is 80-110°C, and the polymerization temperature is also higher, which increases the production cost. ;Use organic solvents as medium, which will pollute the environment; the toxicity of the added amine ligands; after the polymerization of small molecule ligand catalysts of transition metals, the catalysts need to be cumbersomely processed before they can be separated, and the processing cost is too high; difficult to recycle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1. Atom transfer radical polymerization of methyl methacrylate (MMA) in methylimidazole formate ionic liquid ([mim][HCOO])

[0023] Weigh 1 part of CuBr (cuprous bromide, the same below) 3 parts of CuBr 2 (Copper bromide) was dissolved in 500 parts of [mim][HCOO] (methylimidazole formate, the same below) ionic liquid, and nitrogen was passed to remove oxygen. Weigh 500 parts of MMA (methyl methacrylate, the same below) monomer, pass nitrogen to remove oxygen, add to ionic liquid, continue to pass nitrogen to remove oxygen, seal, keep the temperature at 50°C for 20 minutes, inject 1 part of 2 -Ethyl bromoisobutyrate initiator, react at a constant temperature of 50°C. One hour later, the polymerization liquid was treated with methanol to obtain PMMA (polymethyl methacrylate, the same below), Mn=55514, PDI=1.34.

Embodiment 2

[0024] Example 2. Methylimidazole acetate ([mim][CH 3 Atom Transfer Radical Polymerization of Methyl Methacrylate (MMA) in COO]) Ionic Liquid

[0025] Weigh 1 part of CuBr, in 100 parts of [mim][CH 3 COO] dissolved in the ionic liquid, nitrogen in addition to oxygen. Weigh 100 parts of MMA monomer, add nitrogen to remove oxygen, add to ionic liquid, continue to pass nitrogen to remove oxygen, seal, keep the temperature at 50°C for 20 minutes, inject different proportions of initiators, and react at a constant temperature of 50°C. result:

[0026] response a

t / min

Conversion rate / %b

Mnc

Mw / Mn

1d

2e

3f

4g

5h

210

60

60

60

60

62.62

43.28

60.21

65.13

72.61

28428

13653

9723

8583

8018

1.32

1.17

1.17

1.22

1.14

[0027] (In the above table, Mn is the number average molecular weight, Mw is the weight average molecular weight)

[0028] a. All...

Embodiment 3

[0032] Example 3. Polymethyl methacrylate (PMMA) in methylimidazole acetate [mim] [CH 3 COO] ionic liquid, repolymerization in cuprous bromide (CuBr) system

[0033] Weigh 1 part of CuBr, dissolve it in 100 parts of [mim][HCOO] ionic liquid, pass nitrogen to remove oxygen, and keep the temperature at 50°C for 20 minutes. Weigh 0.12 parts of PMMA (Mn=5968) and dissolve it in 100 parts of MMA monomer. After purging nitrogen to remove oxygen, keep the temperature at 50°C for 20 minutes, add it to the ionic liquid, seal it, and react at a constant temperature of 50°C. Result: PMMA with Mn=26533 was obtained.

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Abstract

The invention relates to a method which using new ionic liquor polymerization initiation systerm prepares macromolecular compound. The technical matters of this invention needs to settle is providing a bran-new initiation systerm of atom radical transfer free radical polymerization which using ionic liquor as polymerization medium. The characteristic of this invention's method is the polymerization initiation systerm made up of ionic liquor, initiator and catalysator; the general formula of initiation systerm is [mim][RCOO] / R1X / MXn, the [mim][RCOO] is methyl imidazole organic acid salt ionic liquor, R is alkyl group; R1X is initiator, R1 is alkyl, X is halogen; catalysator MXn is transient metal inorganic salt, n is valence number equal to transition metal; initiation systerm reacts whth monomer can prepare the macromolecular compound of this monomer.

Description

technical field [0001] The invention relates to a method for preparing polymer compounds by adopting a novel ionic liquid polymerization initiation system. The polymerization initiation system is composed of methylimidazole organic acid salt ionic liquid ([mim][RCOO]) as the polymerization medium, R-X as the initiator and low-valence inorganic transition metal salt MXn as the catalyst. The polymerization initiation system does not add any Transition metal organic ligands. Background technique [0002] In 1995, Wang Jinshan first reported in J.Am.chem.Soc., 1995,117,5614 in the atomic group transfer radical polymerization (abbreviated ATRP) initiation system, as initiator is alkyl halide hydrocarbon R-X, wherein X is CI and Br, and R is an organic group with conjugation inducing effect. In the first-generation ATRP initiation system, CuX and organic ligands are mainly used as catalysts. Anbo and Granel in (Macromolecules, 1996, 29: 8576, 1074) used Ru and Ni complexes such ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F20/14C08F12/08C08F4/00C08F297/00
Inventor 胡自强来国桥彭家建邱化玉蒋可志祝根平
Owner HANGZHOU NORMAL UNIVERSITY
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