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Soluble elemental sulfur/terpene copolymer with higher molecular weight and its preparation method and application

A technology of elemental sulfur and copolymer, applied in the field of soluble elemental sulfur/terpene copolymer and its preparation, can solve problems such as application limitation and low molecular weight, and achieve the effects of avoiding waste, high reaction yield and simple operation process

Active Publication Date: 2019-08-20
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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  • Soluble elemental sulfur/terpene copolymer with higher molecular weight and its preparation method and application
  • Soluble elemental sulfur/terpene copolymer with higher molecular weight and its preparation method and application
  • Soluble elemental sulfur/terpene copolymer with higher molecular weight and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A preparation method of elemental sulfur / terpene copolymer, comprising the steps of:

[0041] (1) Add 28g of sublimated sulfur and tetramethyl disulfide to a 150ml four-neck flask equipped with a mechanical stirrer, a condenser, and a thermometer inserted, and heat under nitrogen atmosphere until the sulfur is completely melted, then add 10g of pinene, and heat at 700r / Min speed stirring for about 10min until uniform;

[0042] (2) Heat up the uniformly mixed reaction system in step (1) to 155°C to carry out polymerization reaction. After 2 hours, the product is distilled under reduced pressure for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block 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 fo...

Embodiment 2

[0047] A preparation method of elemental sulfur / terpene copolymer, comprising the steps of:

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

[0049] (2) Heat up the uniformly mixed reaction system in step (1) to 155°C to carry out polymerization reaction. After 2 hours, the product is distilled under reduced pressure for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block 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...

Embodiment 3

[0052] A preparation method of elemental sulfur / terpene copolymer, comprising the steps of:

[0053] (1) Add 28g of sublimated sulfur into a 150ml four-neck flask equipped with a mechanical stirrer, a condenser, and a thermometer inserted into it, add tetramethyl disulfide, heat under a nitrogen atmosphere until the sulfur is completely melted, add 14g of pinene, and heat at 700r / Min speed stirring for about 10min until uniform;

[0054] (2) Heat up the uniformly mixed reaction system in step (1) to 155°C to carry out polymerization reaction. After 2 hours, the product is distilled under reduced pressure for 20 minutes to remove unreacted monomers, and then rapidly cooled and solidified with liquid nitrogen to obtain a dark red block 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°...

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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 in particular relates to a relatively high molecular weight soluble elemental sulfur / terpene copolymer and its preparation method and application. 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. At present, it is mainly used in the chemical industry, such as sulfuric acid and vulcanizing agent. However, the polymeric 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. change. The most important application of insoluble sulfur at present is as a vulcanizing agent for rubber vulcanization. Terpenes, as renewable natural products, are als...

Claims

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Application Information

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Patent Type & Authority Patents(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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