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Preparation method of insoluble sulfur

A sulfur and soluble technology, which is applied in the field of insoluble sulfur preparation, can solve the problems of low content of insoluble sulfur, poor thermal stability and storage stability of insoluble sulfur, and achieve the effects of ensuring thermal stability, reducing sensitivity and ensuring application effect

Pending Publication Date: 2022-04-15
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] One of the purposes of the present invention is to provide a preparation method of insoluble sulfur for the relatively poor thermal stability and storage stability of insoluble sulfur prepared in the prior art. The present invention intends to add Specific types of stabilizers are addressed
[0010] The second object of the present invention is to provide a preparation method of insoluble sulfur for the low content of insoluble sulfur produced by the low-temperature melting method in the prior art. Stabilizers, specific types of dispersants, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] A kind of preparation method of stabilizer for insoluble sulfur preparation, concrete steps are as follows:

[0070] (1) Preparation of raw materials:

[0071] Lithium thiophenyl solution: According to the mass volume ratio of 1g:10mL, lithium thiomethyl was added to tetrahydrofuran to prepare a lithium thiophenyl solution;

[0072] Chloromethyl phenylene sulfide solution: according to the mass volume ratio of 1g:10mL, chloromethyl phenyl sulfide was added to toluene to prepare a chloromethyl phenyl sulfide solution;

[0073] Palladium catalyst: bis(tri-tert-butylphosphine) palladium;

[0074] (2) Add the lithium phenylthiomethyl solution dropwise into the chloromethyl phenyl sulfide solution, and drop it off within 10 minutes, then add the palladium catalyst, stir evenly, and react at a temperature of 25°C for 3 hours to obtain stabilizer A ; Wherein, the mol ratio of lithium phenylthiomethyl and chloromethyl phenyl sulfide is 0.9:1; the addition of palladium catalys...

Embodiment 2

[0077] A kind of preparation method of stabilizer for insoluble sulfur preparation, concrete steps are as follows:

[0078] (1) Preparation of raw materials:

[0079] Lithium thiophenyl solution: According to the mass volume ratio of 1g:11mL, lithium thiomethyl was added to tetrahydrofuran to prepare a lithium thiophenyl solution;

[0080] Chloromethyl phenylene sulfide solution: According to the mass volume ratio of 1g:11mL, chloromethyl phenyl sulfide was added to toluene to prepare a chloromethyl phenyl sulfide solution;

[0081] Palladium catalyst: bis(tri-tert-butylphosphine) palladium;

[0082] (2) Add the lithium phenylthiomethyl solution dropwise into the chloromethyl phenylene sulfide solution, and drop it off within 10 minutes, then add the palladium catalyst, stir evenly, and react at a temperature of 25°C for 4 hours to obtain stabilizer A ; Wherein, the mol ratio of lithium phenylthiomethyl and chloromethyl phenyl sulfide is 0.9:1; the addition of palladium cata...

Embodiment 3

[0085] A kind of preparation method of stabilizer for insoluble sulfur preparation, concrete steps are as follows:

[0086] (1) Preparation of raw materials:

[0087] Lithium thiophenyl solution: According to the mass volume ratio of 1g:12mL, lithium thiomethyl was added to tetrahydrofuran to prepare a lithium thiophenyl solution;

[0088] Chloromethyl phenylene sulfide solution: according to the mass volume ratio of 1g:13mL, chloromethyl phenyl sulfide was added to toluene to prepare a chloromethyl phenyl sulfide solution;

[0089] Palladium catalyst: bis(tri-tert-butylphosphine) palladium;

[0090] (2) Add the lithium phenylthiomethyl solution dropwise into the chloromethyl phenyl sulfide solution, and drop it off within 10 minutes, then add the palladium catalyst, stir evenly, and react at a temperature of 25°C for 5 hours to obtain stabilizer A ; Wherein, the mol ratio of lithium phenylthiomethyl and chloromethyl phenyl sulfide is 1:1; the addition of palladium catalyst ...

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Abstract

The invention provides a preparation method of insoluble sulfur. The preparation method comprises the following steps: sequentially performing extraction, drying, sieving and oil filling treatment on an insoluble sulfur semi-finished product to obtain an insoluble sulfur finished product, drying treatment refers to uniformly mixing a product obtained by extraction with a stabilizer and then carrying out vacuum drying; the stabilizer is a stabilizer A or a stabilizer B or a mixture of the stabilizer A and the stabilizer B or a mixture of the stabilizer A and the stabilizer C or a mixture of the stabilizer B and the stabilizer C or a mixture of the stabilizer A, the stabilizer B and the stabilizer C; when the insoluble sulfur semi-finished product is prepared, a low-temperature melting method is adopted, and technological parameters of the reaction and the type of quenching liquid are adjusted; a dispersing agent 1 is added during oil filling treatment. The method provided by the invention is simple, solves the problem of low content of insoluble sulfur prepared by adopting a low-temperature melting method in the prior art, and also solves the problem that the thermal stability and storage stability of the insoluble sulfur prepared by the prior art need to be further improved.

Description

technical field [0001] The invention belongs to the technical field of sulfur production, and in particular relates to a preparation method of insoluble sulfur. Background technique [0002] Insoluble sulfur (abbreviated as IS) is a thermoplastic linear polymer homopolymer, which is non-toxic, flammable, and insoluble in carbon disulfide. Insoluble sulfur is physically and chemically inert, and when used for rubber vulcanization, it can prevent the rubber from blooming and scorching. Therefore, it is often used as a vulcanizing agent for radial tires to improve its wear resistance and service life. However, insoluble sulfur is a metastable substance, and various factors such as high temperature, induction of alkaline substances or long-term storage may cause insoluble sulfur to depolymerize into ordinary sulfur. And ordinary sulfur itself has S 8 Ring structure, S 8 The ring structure is heated and opened to form a chain free radical monomer with unsaturated sulfur atoms ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/12
Inventor 颜志勇胡英钟楚涛王晓馨姚勇波尹岸林张葵花
Owner JIAXING UNIV