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Method for regulating and controlling dispersity of product of reversible addition-fragmentation chain transfer polymerization method

A technology of fragmentation chain transfer and polymerization, which is applied in the field of reversible addition-fragmentation chain transfer polymerization, can solve the problems of not being diblock copolymers, etc., and achieve the effects of wide control range, easy use, and simple operation

Active Publication Date: 2020-09-08
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although block copolymers can be prepared, but the chain is doped with a certain amount of butyl acrylate, it is not a pure diblock copolymer

Method used

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  • Method for regulating and controlling dispersity of product of reversible addition-fragmentation chain transfer polymerization method
  • Method for regulating and controlling dispersity of product of reversible addition-fragmentation chain transfer polymerization method
  • Method for regulating and controlling dispersity of product of reversible addition-fragmentation chain transfer polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment one does not add chain terminator synthetic polymethyl methacrylate (PMMAS)

[0049] Multiple groups of experiments were carried out in parallel, and each group of experiments reacted at different times. The specific method is as follows:

[0050] Moore, [MMA] 0 :[MBr] 0 :[CPDB] 0 :[ACCN] 0 =200:0:1:0.2, sequentially add CPDB (0.0209g), ACCN (0.0046g), MMA (2.0mL) and DMF (2.0mL) in the 10mL ampoule, add a stirring bar, after 3 times of standard After the freeze-pump-thaw aeration cycle, seal the tube under an oxygen-free atmosphere. The sealed ampoule was placed in a magnetic stirrer at 110° C. for a predetermined time and the rotation speed was 600 rpm. After the reaction, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of methanol, leave it overnight, filter it with suction, and dry it to obtain polymethyl methacrylate (PMMA).

[0051] figure 1 For not adding under the condition of chai...

Embodiment 2

[0054] Example two sample molar ratio monomer: chain terminator: chain transfer agent=200:5:1 synthetic polymethyl methacrylate

[0055] Multiple groups of experiments were carried out in parallel, and each group of experiments reacted at different times. The specific method is as follows:

[0056] Moore, [MMA] 0 :[MBr] 0 :[CPDB] 0 :[ACCN] 0 =200:5:1:0.2, sequentially add MBr (0.0830g), CPDB (0.0209g), ACCN (0.0046g), MMA (2.0mL) and DMF (2.0mL) in a 10mL ampoule, add a stirring bar , after 3 standard freeze-pump-thaw inflation cycles, seal the tube under an oxygen-free atmosphere. The sealed ampoule was placed in a magnetic stirrer at 110° C. for a predetermined time and the rotation speed was 600 rpm. After the reaction is over, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of methanol, leave it overnight, filter it with suction, and dry it to obtain polymethyl methacrylate.

[0057] image 3 For adding...

Embodiment 3

[0060] Embodiment three sample molar ratio monomer: chain terminator: chain transfer agent=200:10:1 synthetic polymethyl methacrylate

[0061] Multiple groups of experiments were carried out in parallel, and each group of experiments reacted at different times. The specific method is as follows:

[0062] Moore, [MMA] 0 :[MBr] 0 :[CPDB] 0 :[ACCN] 0 =200:10:1:0.2, sequentially add MBr (0.1660g), CPDB (0.0209g), ACCN (0.0046g), MMA (2.0mL) and DMF (2.0mL) to a 10mL ampoule, add a stir bar , after 3 standard freeze-pump-thaw inflation cycles, seal the tube under an oxygen-free atmosphere. The sealed ampoule was placed in a magnetic stirrer at 110° C. for a predetermined time and the rotation speed was 600 rpm. After the reaction is over, take out the sealed tube, open the sealed tube, dissolve it with 2-5 mL of tetrahydrofuran, pour it into 250 mL of methanol, leave it overnight, filter it with suction, and dry it to obtain polymethyl methacrylate.

[0063] Figure 5 For ad...

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Abstract

The invention relates to a method for regulating and controlling the dispersity of a product of a reversible addition-fragmentation chain transfer polymerization method. The method comprises the following steps that: in the presence of a chain terminator, vinyl monomers are subjected to RAFT polymerization reaction in an organic solvent under the action of a chain transfer agent and an initiator,when the chain terminator is 2-bromo maleimide, a reversible addition-fragmentation chain transfer polymerization reaction is carried out at the constant temperature of 40-110 DEG C, when the chain terminator is furan-protected 2-bromo maleimide, and the reversible addition-fragmentation chain transfer polymerization reaction is carried out under a program variable temperature condition, wherein the program variable temperature condition is that the reaction is carried out at 40 DEG C and then at least one temperature higher than 40 DEG C. According to the method, the product with the target dispersity can be obtained only by additionally adding a small amount of chain terminator in RAFT polymerization, the reaction operation is simple, and the substrate applicability is wide.

Description

technical field [0001] The invention relates to the field of reversible addition-fragmentation chain transfer polymerization, in particular to a method for regulating the dispersion degree of products in the reversible addition-fragmentation chain transfer polymerization method. Background technique [0002] Polydispersity has a profound effect on the glass transition temperature of polymers, viscosity, processability, and self-assembly behavior of block copolymers. It has been demonstrated that triblock polymers with polydisperse in the middle or at both ends can form a completely different phase diagram from monodisperse polymers. In industrial production, polydisperse polyethylene is used to make tires. Its high molecular weight part ensures sufficient elasticity, while the low molecular weight part has low viscosity, which improves the processability of the material. [0003] At present, there are mainly the following methods for preparing polydisperse polymers: [000...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08F2/38C08F2/42C08F112/08
CPCC08F2/38C08F2/42C08F112/08C08F120/14C08F2438/03
Inventor 黄智豪贾睿张正彪
Owner SUZHOU UNIV
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