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Preparation method of macromolecular crosslinking agent for ultraviolet light crosslinking polyolefin

A technology of macromolecular crosslinking agent and crosslinking polyolefin, which is applied in the field of preparation of macromolecular crosslinking agent, can solve the problems of easy volatilization and migration, reduction of crosslinking efficiency, pollution of the environment, etc., and achieve high molecular weight and high conversion rate , Easy to operate

Active Publication Date: 2014-12-10
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crosslinking agent used also has a high vapor pressure at the processing temperature, which is easy to volatilize and migrate, resulting in a decrease in crosslinking efficiency and polluting the environment.

Method used

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  • Preparation method of macromolecular crosslinking agent for ultraviolet light crosslinking polyolefin
  • Preparation method of macromolecular crosslinking agent for ultraviolet light crosslinking polyolefin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under the conditions of nitrogen atmosphere and ice-water bath, 30g 1,6-hexanediol bis(2-mercaptoacetate) and 70.2g triallyl isocyanate were dissolved in 76g toluene respectively, mixed and stirred evenly And add 1.0g of azobisisobutyronitrile, slowly heated to 65 ° C reaction, until the infrared spectrum on the 2570cm -1 The characteristic peak of the mercapto group disappears; after the reaction, the solvent is evaporated to dryness to obtain an allyl-type macromolecular cross-linking agent.

[0027] figure 1 It is the infrared spectrogram of the macromolecular crosslinking agent used for ultraviolet light crosslinking polyolefin prepared in this embodiment. Depend on figure 1 It can be seen that 2570cm -1 The characteristic absorption peak of the sulfhydryl group disappears, indicating that the dithiol compound is completely consumed; 3082cm -1 ,993cm -1 It is the absorption peak of the C-H bond on the allyl group, 2943cm -1 It is the absorption peak of the C-H...

Embodiment 2

[0035] Under nitrogen atmosphere and room temperature, 20g 1,4-butanediol bis(3-mercaptopropionate) and 57.3g trimethylolpropane triallyl ether were dissolved in 77g acetonitrile respectively, mixed and stirred evenly and Add 1.55g benzoin dimethyl ether, at 20mw / cm 2 Under the irradiation of ultraviolet lamp, the reaction is carried out until 2570cm on the infrared spectrum -1 The characteristic peak of the mercapto group disappears; after the reaction, the solvent is evaporated to dryness to obtain an allyl-type macromolecular cross-linking agent.

[0036] The molecular weight and distribution of the macromolecular crosslinking agent prepared in this example were measured by gel permeation chromatography, and the number average molecular weight was measured to be 3800, and the molecular weight distribution was 2.1. It can be seen that the molecular weight of the macromolecular crosslinking agent prepared in this example is much larger than that of the small molecular crossl...

Embodiment 3

[0042] Under the condition of nitrogen atmosphere and ice-water bath, 30g triethylene glycol bis(2-mercaptoacetate) and 33.5g pentaerythritol triallyl ether were respectively dissolved in 95g xylene, mixed and stirred evenly and added 0.51 g benzoyl peroxide, slowly heated to 70 ° C to react until 2570 cm on the infrared spectrum -1 The characteristic peak of the mercapto group disappears; after the reaction, the solvent is evaporated to dryness to obtain an allyl-type macromolecular cross-linking agent.

[0043] The molecular weight and distribution of the macromolecular crosslinking agent prepared in this example were measured by gel permeation chromatography, and the number average molecular weight was measured to be 7300, and the molecular weight distribution was 1.9. It can be seen that the molecular weight of the macromolecular crosslinking agent prepared in this example is much larger than that of the small molecular crosslinking agent pentaerythritol triallyl ether (it...

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Abstract

The invention discloses a preparation method of a macromolecular crosslinking agent for ultraviolet light crosslinking polyolefin. The preparation method comprises the steps of adding a dimercapto compound, an allyl crosslinking agent and an initiator into a solvent for reaction under a nitrogen shielding condition till a characteristic peak of a sulfhydryl group at 2570cm<-1> on an infrared spectrum disappears, removing the solvent after the reaction, and obtaining the macromolecular crosslinking agent in a hyperbranched structure. Compared with a micromolecular crosslinking agent, the molecular weight of the macromolecular crosslinking agent is obviously increased; volatility is reduced significantly at the same operating temperature; and at the same time, due to the uniqueness of the hyperbranched structure, the macromolecular crosslinking agent has many end groups and a good crosslinking effect. The preparation method is mild in reaction condition, high in conversion rate and easy and simple to operate, effectively solves the problems of the volatility and mobility of the micromolecular crosslinking agent in a storage and processing procedure of ultraviolet light crosslinking polyolefin, and has higher crosslinking efficiency and good compatibility with polyolefin.

Description

1. Technical field [0001] The invention relates to a macromolecular crosslinking agent, in particular to a preparation method of the macromolecular crosslinking agent used for ultraviolet light crosslinking polyolefin. 2. Background technology [0002] Polyolefin is the most widely used general-purpose thermoplastic polymer material among polymer materials, and plays a huge role in national economic construction and daily life. However, polyolefins generally have low softening points and mechanical strengths, limiting their applications. The most effective way to improve the performance of polyolefin is to promote its crosslinking to form a three-dimensional network structure, which will significantly increase its service temperature and enhance its resistance to stress cracking. Cross-linked polyolefins have become increasingly important and widely used polymeric materials. [0003] Ultraviolet light cross-linking is a newest method for producing cross-linked polyolefin d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00C08L23/06C08L87/00C08J3/28C08J3/24
Inventor 谢寒吴强华施文芳瞿保钧
Owner UNIV OF SCI & TECH OF CHINA
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