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A kind of butene graft polyethylene glycol copolymer and preparation method thereof

A grafted polyethylene glycol and butene copolymerization technology, applied in the field of polybutene research, can solve the problems of polymer crystallinity reduction, polybutene main chain regularity damage, crystallization ability decline, etc.

Inactive Publication Date: 2021-06-22
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of butene graft polyethylene glycol copolymer and preparation method thereof
  • A kind of butene graft polyethylene glycol copolymer and preparation method thereof
  • A kind of butene graft polyethylene glycol copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0067]

[0068] The molecular weight of the grafted PEG segment is 750 g / mol.

[0069] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0070] 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);

[0071] 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 (0.4ml) ]-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 complet...

Embodiment 2

[0077] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0078]

[0079] The molecular weight of the grafted PEG segment is 2000 g / mol.

[0080] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0081] 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);

[0082] 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 (0.4ml) ]-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 3

[0088] The butene graft polyethylene glycol copolymer of the present embodiment has a structure as shown in the following formula;

[0089]

[0090] The molecular weight of the grafted PEG segment is 4000g / mol.

[0091] Described novel butene graft polyethylene glycol copolymer is prepared through following method:

[0092] 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);

[0093] 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 (0.4ml) ]-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 complet...

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Abstract

The invention relates to a butene-grafted polyethylene glycol copolymer and a preparation method thereof. A coordination polymerization catalyst is used to catalyze the polymerization of butene and a comonomer containing a trimethylsilyl group to obtain a copolymer, and then use it as an intermediate The polybutene grafted with polyethylene glycol segments of different molecular weights was prepared by reacting the body with polyethylene glycol after azidation at one end. At the same time, the same catalyst was used to prepare polybutenes with molecular weights and molecular weight distributions close to those of copolymers. butene homopolymer for comparison. By grafting polyethylene glycol with different molecular weights onto the polybutene main chain, the crystallization ability and crystallinity of the copolymer are improved, and the crystallization temperature of the graft copolymer even exceeds that of the homopolymer. At the same time, the phase transition rate of the sample is also different from the previous understanding. The phase transition rate of the copolymer grafted with lower molecular weight PEG is faster than that of the homopolymer, which provides a new insight for the subsequent research on the polybutene system. train of thought.

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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Patent Type & Authority Patents(China)
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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