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A kind of soluble elemental sulfur/alicyclic olefin copolymer and preparation method thereof

A technology of alicyclic olefin and elemental sulfur, which is applied in the field of elemental sulfur/alicyclic olefin copolymer and its preparation, can solve the problems of poor stabilization effect of stabilizer, impossibility of material processing and use, and small amount of stabilizer added. The effects of low toxicity, low reaction temperature and high product yield

Active Publication Date: 2017-11-10
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of conventional stabilizer added is very small, accounting for about 0.1% to 1% of the mass of sulfur, and it is only used as an additive. The polymerized sulfur obtained in this way is not only insoluble in any solvent, but also has a low yield. The stabilization effect is also not good, and it cannot be used as a material for processing

Method used

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  • A kind of soluble elemental sulfur/alicyclic olefin copolymer and preparation method thereof
  • A kind of soluble elemental sulfur/alicyclic olefin copolymer and preparation method thereof
  • A kind of soluble elemental sulfur/alicyclic olefin copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1 contains the polysulfur copolymer of 10wt% limonene

[0050] (1) First add 9g of sublimed sulfur into a 50mL three-necked flask without catalyst, 2Heat to 120°C under atmosphere, after the sulfur is completely melted, add 1g limonene, and stir at 600r / min for 5min until uniform;

[0051] (2) Warm up the uniformly mixed reaction system in step (1) to 250°C to carry out polymerization reaction. After 0.5h of polymerization reaction, pour the product into liquid nitrogen and quickly cool it to room temperature to solidify, that is, the polymerization The crude product of the sulfur copolymer; then the purification of the crude product of the polymerized sulfur copolymer is carried out by precipitation method: the crude product of the obtained polymerized sulfur copolymer is dissolved in tetrahydrofuran to saturation, filtered, and the filtrate is added to anhydrous Precipitate in ethanol for 15 minutes, then filter the obtained suspension under reduced pressu...

Embodiment 2

[0052] Example 2 Polymerized sulfur copolymer containing 30 wt% limonene

[0053] (1) First add 7g of sublimed sulfur in a 50mL three-necked flask, add 0.5wt% (0.5% of the mass of elemental sulfur) of hexamethylenetetramine, and 2 Heating to 158°C under atmosphere, after the sulfur is completely melted, add 3g of limonene, and stir at a speed of 450r / min for 5min until uniform;

[0054] (2) Warm up the uniformly mixed reaction system in step (1) to 180°C to carry out polymerization reaction. After 1 hour of polymerization reaction, pour it into liquid nitrogen and quickly cool it to room temperature to solidify, that is, the polymerized sulfur copolymer in the form of an orange-red blocky solid is obtained. Then use the precipitation method to carry out the purification of the crude product of the polymerized sulfur copolymer: dissolve the crude product of the obtained polymerized sulfur copolymer in dichloromethane to saturation, filter, and add the filtrate to isopropyl alco...

Embodiment 3

[0055] Example 3 Polymerized sulfur copolymer containing 50 wt% limonene

[0056] (1) First add 5g of sublimed sulfur in a 50mL there-necked flask, add 1wt% (1% of the mass of elemental sulfur) of ammonium persulfate, and 2 Heat to 158°C under atmosphere, after the sulfur is completely melted, add 5g limonene, and stir at a speed of 300r / min for 10min until uniform;

[0057] (2) Heat the uniformly mixed reaction system in step (1) to the boiling point of limonene, that is, 177°C, and carry out polymerization reaction. After 6 hours of polymerization reaction, pour it into liquid nitrogen and quickly cool it to room temperature to solidify, and a red blocky solid is obtained. The crude product of polymerized sulfur copolymer. Then adopt the precipitation method to carry out the purification of the crude product of the polymerized sulfur copolymer: dissolve the crude product of the obtained polymerized sulfur copolymer in pyridine to saturation, filter, add the filtrate to meth...

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Abstract

The invention belongs to the field of chemical synthesis, and in particular relates to a soluble elemental sulfur / alicyclic olefin copolymer and a preparation method thereof. In the present invention, the elemental sulfur is heated in the N2 atmosphere under the condition of catalyst presence or absence until the temperature of the reaction system is above the melting point of the elemental sulfur and below the transition temperature. After the elemental sulfur is completely melted, the alicyclic olefin monomer is added and stirred. Mix evenly; then perform polymerization reaction to obtain soluble elemental sulfur / alicyclic olefin copolymer; the copolymer introduces carbon chains in the sulfur chain, which not only eliminates sulfur free radicals, but also because the unsaturated olefin used contains more than one The double bond can act as a chemical cross-linking point, which in turn can stabilize the sulfur chain.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a soluble elemental sulfur / alicyclic olefin copolymer and a preparation method thereof. Background technique [0002] As a by-product of hydrodesulfurization in the petroleum refining process in the petrochemical industry, sulfur has an annual output of tens of millions of tons, but its application range is very limited. Its industrial use is mainly to prepare sulfuric acid, dyes and rubber vulcanizing agents. Although sulfur raw materials are very abundant, there is almost no domestic sulfur-rich polymer materials that can be converted into sulfur-rich polymer materials. It is well known that elemental sulfur is mainly formed as the most stable 8-membered ring (S 8 ) form, but under the condition of heating, the crystal form will change from orthorhombic sulfur to monoclinic sulfur. When the temperature reaches 120-124 ° C, it will melt and transform into a liquid ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C01B17/12
Inventor 许凯孙龙凤任圆圆林伟鸿彭军邢玉秀高树曦陈鸣才
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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