High-molecular-weight soluble elementary sulfur/terpene copolymer, and preparation method and application of same

A technology of elemental sulfur and copolymer, applied in the field of soluble elemental sulfur/terpene copolymer and its preparation, can solve the problems of low molecular weight and application limitation, and achieve the effects of high reaction yield, avoidance of waste and easy experimental conditions

Active Publication Date: 2017-12-22
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its low molecular weight (generally less than 10 3 ), the application is limited

Method used

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  • High-molecular-weight soluble elementary sulfur/terpene copolymer, and preparation method and application of same
  • High-molecular-weight soluble elementary sulfur/terpene copolymer, and preparation method and application of same
  • High-molecular-weight soluble elementary sulfur/terpene copolymer, and preparation method and application of same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A method for preparing elemental sulfur / terpene copolymer includes the following steps:

[0041] ⑴ Put 28g of sublimed sulfur into a 150ml four-necked flask equipped with mechanical stirring, condenser and thermometer inserted, add tetramethyl disulfide, and heat under nitrogen atmosphere until the sulfur is completely melted, add 10g pinene, and add 700r / Stir at a speed of about 10 minutes until it is uniform;

[0042] (2) Raise the uniformly mixed reaction system in step (1) to 155°C to carry out the polymerization reaction. After 2 hours, the product is subjected to vacuum distillation for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block. The solid polymerized sulfur crude product; the crude product is dissolved in tetrahydrofuran, filtered and centrifuged to remove insoluble impurities; then the solvent is removed by rotary evaporation, and then placed in a vacuum drying oven at 40°C for 12 h...

Embodiment 2

[0047] A method for preparing elemental sulfur / terpene copolymer includes the following steps:

[0048] ⑴ Put 28g of sublimed sulfur into a 150ml four-necked flask equipped with mechanical stirring, condenser and thermometer inserted, add ammonium persulfate, and heat it under nitrogen atmosphere until the sulfur is completely melted, then add 10g of pinene, and add 10g of pinene at 700r / min. Stir at a speed of about 10min to uniform;

[0049] (2) Raise the uniformly mixed reaction system in step (1) to 155°C to carry out the polymerization reaction. After 2 hours, the product is subjected to vacuum distillation for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block. The solid polymerized sulfur crude product; the crude product is dissolved in tetrahydrofuran, filtered and centrifuged to remove insoluble impurities; then the solvent is removed by rotary evaporation, and then placed in a vacuum drying oven ...

Embodiment 3

[0052] A method for preparing elemental sulfur / terpene copolymer includes the following steps:

[0053] ⑴ Put 28g of sublimed sulfur into a 150ml four-necked flask equipped with mechanical stirring, condenser and thermometer inserted, add tetramethyl disulfide, and heat under nitrogen atmosphere until the sulfur is completely melted, add 14g pinene, and add 700r / Stir at a speed of about 10 minutes until it is uniform;

[0054] (2) Raise the uniformly mixed reaction system in step (1) to 155°C to carry out the polymerization reaction. After 2 hours, the product is subjected to vacuum distillation for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block. The solid polymerized sulfur crude product; the crude product is dissolved in tetrahydrofuran, filtered and centrifuged to remove insoluble impurities; then the solvent is removed by rotary evaporation, and then placed in a vacuum drying oven at 40°C for 12 h...

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Abstract

The invention discloses a high-molecular-weight soluble elementary sulfur/terpene copolymer, and a preparation method and an application of same. The preparation method includes the following steps: 1) heating elementary sulfur in nitrogen gas and a vulcanization accelerator until the elementary sulfur is fused completely, adding terpene, and uniformly mixing the components; 2) increasing temperature of the reaction system to 150-240 DEG C to perform a reaction for 0.5-6.0 h, and purifying a product to obtain a sulfur-rich oligomer; 3) dissolving the sulfur-rich oligomer and removing oxygen, adding an oxidant to perform a reaction at 20-80 DEG C for 0.5-8.0 h, and purifying the product to prepare the elementary sulfur/terpene copolymer. The invention, for the first time, discloses a process of synthesizing the high-molecular-weight soluble elementary sulfur/terpene copolymer from sulfur and terpene, and overcomes the defect that an elementary sulfur/terpene copolymer in the prior art is low in molecular weight and is limited in application. The raw materials in the invention are low in cost and easy to obtain; by means of the sulfur, resource waste is effectively avoided. The preparation method has simple processes, employs easy experimental conditions, and is high in reaction yield.

Description

Technical field [0001] The invention belongs to the field of chemical synthesis, and specifically relates to a higher molecular weight soluble elemental sulfur / terpene copolymer, and a preparation method and application thereof. Background technique [0002] As we all know, sulfur is a by-product of the petrochemical industry and its annual output is increasing year by year, but its utilization rate is very limited. It is currently mainly used in the chemical industry, such as sulfuric acid and vulcanizing agents. However, the polymerized sulfur (also called insoluble sulfur) obtained by directly thermally polymerizing sulfur is thermodynamically unstable, has a low conversion yield, and is insoluble in any organic solvent, so it is necessary to find a substance to copolymerize with it to stabilize it. 化. The main application of insoluble sulfur currently is as a vulcanizing agent for rubber vulcanization. As a renewable natural product, terpenes are mainly used as solvents. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F132/08C08K3/06C08L45/00
Inventor 许凯孙龙凤邢玉秀高树曦桂雪峰梁晟源陈鸣才
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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