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Butene grafted polyethylene glycol copolymer and preparation method thereof

A technology of grafting polyethylene glycol and copolymers, which is applied in the field of polybutene research, can solve the problems of polybutene main chain regularity damage, polymer crystallinity reduction, crystallization ability decline, etc., and achieves ingenious polymerization methods, The effect of narrow molecular weight distribution and high isotacticity

Inactive Publication Date: 2019-07-23
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, even if it is a copolymerization that promotes phase transition, the introduction of copolymerization units also has some disadvantages, which will destroy the regularity of the main chain of polybutene, reduce the crystallinity of the polymer, and reduce the crystallization ability.

Method used

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  • Butene grafted polyethylene glycol copolymer and preparation method thereof
  • Butene grafted polyethylene glycol copolymer and preparation method thereof
  • Butene grafted polyethylene glycol copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0066]

[0067] The molecular weight of the grafted PEG segment is 750 g / mol.

[0068] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0069] 1) Weigh 15 μmol of dimethylsilyl-bridged zirconocene catalyst, 30 μmol of cocatalyst borane and 100 mL of ultra-dry toluene for use (the total polymerization system is 90 ml);

[0070] 2) Under anhydrous and oxygen-free conditions, feed 1MPa butene gas into the reactor, and then add 4-[4-(trimethylsilylethynyl)-phenyl with a concentration of 20mmol / L (0.4 ml) ]-1-butene comonomer, and then add 70ml of ultra-dry toluene as a solvent, then add 100 times the amount of catalyst material triisobutylaluminum as a chain transfer agent in the system, and then use 10ml of ultra-dry Toluene dissolves the catalyst and co-catalyst. After the dissolution is comple...

Embodiment 2

[0076] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0077]

[0078] The molecular weight of the grafted PEG segment is 2000 g / mol.

[0079] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0080] 1) Weigh 15 μmol of dimethylsilyl-bridged zirconocene catalyst, 30 μmol of cocatalyst borane and 100 mL of ultra-dry toluene for use (the total polymerization system is 90 ml);

[0081] 2) Under anhydrous and oxygen-free conditions, feed 1MPa butene gas into the reactor, and then add 4-[4-(trimethylsilylethynyl)-phenyl with a concentration of 20mmol / L (0.4 ml) ]-1-butene comonomer, and then add 70ml of ultra-dry toluene as a solvent, then add 100 times the amount of catalyst material triisobutylaluminum as a chain transfer agent in the system, and then use 10ml of ultra-dry Toluene dissolves the catalyst and co-catalyst. After the dissolution is compl...

Embodiment 3

[0087] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0088]

[0089] The molecular weight of the grafted PEG segment is 4000g / mol.

[0090] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0091] 1) Weigh 15 μmol of dimethylsilyl-bridged zirconocene catalyst, 30 μmol of cocatalyst borane and 100 mL of ultra-dry toluene for use (the total polymerization system is 90 ml);

[0092] 2) Under anhydrous and oxygen-free conditions, feed 1MPa butene gas into the reactor, and then add 4-[4-(trimethylsilylethynyl)-phenyl with a concentration of 20mmol / L (0.4 ml) ]-1-butene comonomer, and then add 70ml of ultra-dry toluene as a solvent, then add 100 times the amount of catalyst material triisobutylaluminum as a chain transfer agent in the system, and then use 10ml of ultra-dry Toluene dissolves the catalyst and co-catalyst. After the dissolution is comple...

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Abstract

The invention relates to a butene grafted polyethylene glycol copolymer and a preparation method thereof. Coordination polymerization catalyst catalytic butene and a comonomer containing a trimethyl silicon group are polymerized to obtain the copolymer; then, the copolymer is taken as an intermediate to react with polyethylene glycol of which one end is subjected to azidation to prepare polybutylene which grafts polyethylene glycol chain segments with different molecular weights; meanwhile, the same catalyst is used for preparing a butene homopolymer of which the molecular weight and the molecular weight distribution are similar to those of the copolymer for comparing. Polyethylene glycol grafted with different molecular weights is prepared on a polybutylene main chain. Compared with the copolymer, the butene grafted polyethylene glycol copolymer has the advantages that the crystallization capacity and a degree of crystallinity are improved, in addition, the crystallization temperatureof the grafted copolymer even exceeds the crystallization temperature of a homopolymer, meanwhile, a phase transformation rate of a sample is different from previous understanding, the phase transformation rate of the copolymer grafted with PEG (polyethylene glycol) of low molecular weight is quicker than the phase transformation rate of the homopolymer, and a new thought is provided for subsequent researches about a polybutylene system.

Description

technical field [0001] The invention relates to the field of polybutene research, and relates to a butene-grafted polyethylene glycol copolymer and a preparation method thereof. Background technique [0002] Polybutene is a polymer material with excellent creep resistance, good environmental stress crack resistance, good heat resistance, high hardness and other excellent properties, known as "plastic gold". At the same time, polybutene is also a very typical semi-crystalline polymer, and there are four different crystal structures, namely form I, form I', form II and form III. Among them, formI and form I' have 3 1 The hexagonal phase crystal with helical structure is also the most thermodynamically stable crystal form of polybutene. The formation conditions of these two crystal forms are different, form I' is formed directly from the melt or solution, and form I is generally obtained from the metastable tetragonal phase crystal form II through solid-solid phase transforma...

Claims

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Application Information

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IPC IPC(8): C08G81/02C08F210/08C08F230/08
CPCC08F210/08C08G81/025C08F230/08
Inventor 李悦生李玉莲安传斌马哲
Owner TIANJIN UNIV
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