Method for preparing sulfur-rich polymer at room temperature through mechanochemically induced reverse vulcanization reaction

A sulfur-rich polymer, mechanochemical technology, applied in the field of material chemistry, can solve the problems of low boiling point small molecule comonomers, such as high reaction temperature and inability to react.

Active Publication Date: 2022-01-14
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic reverse vulcanization does not solve the problem that low-boiling point small molecule comonomers cannot react due to high reaction temperature. ...

Method used

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  • Method for preparing sulfur-rich polymer at room temperature through mechanochemically induced reverse vulcanization reaction
  • Method for preparing sulfur-rich polymer at room temperature through mechanochemically induced reverse vulcanization reaction
  • Method for preparing sulfur-rich polymer at room temperature through mechanochemically induced reverse vulcanization reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Weigh 2.5g of sulfur elemental powder, 2.5g of dicycloheptadiene and 50.0mg of barium titanate in a 50ml cylinder of a vertical planetary ball mill, and react at room temperature for 6 hours at a speed of 300r / min. After the reaction is completed, , taken out with a spatula to obtain a sulfur-rich polymer. Characterized by XRD, the conversion rate of sulfur element is about 100%, and the hydrogen sulfide gas generation is less than 20ppm.

Embodiment 2

[0029] (2) Weigh 2.5g of sulfur elemental powder, 2.5g of 1,3-divinylbenzene and 50.0mg of barium titanate into a 50ml cylinder of a vertical planetary ball mill, and react at room temperature for 6 hours at a rotational speed of 300r / min. After the end, take out with a spatula to obtain the sulfur-rich polymer. Characterized by XRD, the conversion rate of sulfur element is about 100%, and the hydrogen sulfide gas generation is less than 20ppm.

Embodiment 3

[0031] (3) Weigh 2.5g of sulfur elemental powder, 2.5g of squalene and 50.0mg of barium titanate in a 50ml cylinder of a vertical planetary ball mill, and react at room temperature for 6 hours at a speed of 300r / min. After the reaction is completed, use The scraper was taken out to obtain the sulfur-rich polymer. Characterized by XRD, the conversion rate of sulfur element is about 100%, and the hydrogen sulfide gas generation is less than 20ppm.

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Abstract

The invention discloses a method for preparing a sulfur-rich polymer at room temperature through mechanochemically induced reverse vulcanization polymerization. The polymerization method comprises the following steps: mixing elemental sulfur, a micromolecular comonomer and a catalyst, and carrying out a room temperature reaction in mechanochemical equipment for a certain time to prepare the sulfur-containing polymer, wherein the elemental sulfur and a cross-linking agent are mixed according to a mass ratio of 5: 95 to 95: 5, and the amount of the catalyst is 0-10% by mass. The synthesis method provided by the invention overcomes the high-temperature condition required by traditional reverse vulcanization, not only reduces the energy consumption, improves the product yield and reduces the generation of a by-product hydrogen sulfide in the reaction process, but also expands the range of monomers suitable for reverse vulcanization polymerization, and provides a safe and clean chemical conversion method for converting waste sulfur into functional plastics.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to a method for preparing a sulfur-rich polymer at room temperature through a mechanochemically induced reverse vulcanization reaction. Background technique [0002] Polymers are widely present in human society. But the vast majority of polymers are produced from finite resources in petrochemicals, so the cost of synthetic polymer raw materials and their sustainability must be considered. Sulfur is an underutilized by-product of the petrochemical industry. The hydrodesulfurization process of crude oil and natural gas produces more than 70 million tons of sulfur per year. The supply far exceeds demand, resulting in a large sulfur surplus. Therefore, as a raw material that can replace polymer material carbon, it has great application potential. [0003] Although sulfur alone can undergo ring-opening polymerization at high temperature, the resulting polymer is unstable a...

Claims

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Application Information

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IPC IPC(8): C08G75/16
CPCC08G75/16
Inventor 贺丽蓉赵辉杨东张楚虹
Owner SICHUAN UNIV
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