Method for preparing insoluble sulfur through blocking molecular chain of quenching polymerization product of sulfur monomer

A molecular chain and quenching technology, applied in the preparation/purification of sulfur, etc., can solve the problems of extensive formation of polymerized sulfur, unsatisfactory thermal stability and dispersibility of products, etc., to avoid poor product stability, improve labor environment, The effect of reducing labor intensity

Inactive Publication Date: 2017-09-26
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the technical problems of the insoluble sulfur production process in the prior art, such as the extensive formation of polymerized sulfur and the unsatisfactory thermal stability and dispersibility of the product, the purpose of the present invention is to provide a sulfur monomer quenched polymerization product molecular chain capping preparation Insoluble Sulfur Method

Method used

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  • Method for preparing insoluble sulfur through blocking molecular chain of quenching polymerization product of sulfur monomer
  • Method for preparing insoluble sulfur through blocking molecular chain of quenching polymerization product of sulfur monomer
  • Method for preparing insoluble sulfur through blocking molecular chain of quenching polymerization product of sulfur monomer

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Effect test

Embodiment 1

[0032] The method for preparing insoluble sulfur by capping the molecular chain of sulfur monomer quenching polymerization product, specifically includes the following steps:

[0033] In the first step, after the solid sulfur is melted, the temperature is raised to 130°C, and gradually gasified to 550°C.

[0034] In the second step, the sulfur vapor vaporized in the first step is sprayed into the tank at a speed of 300Kg / hr through the nozzle, and the temperature is 25 ° C, the sulfur mass ratio is 45:1, and contains 0.02 parts by weight of ferric chloride, The aqueous solution of 0.03 parts by weight of nitric acid is atomized and contacted, and cooled; the formed pseudoplastic is powder, the particle size distribution is less than 100 mesh, and the content is 98%, and the intermediate contains 55% of insoluble sulfur.

[0035] In the third step, the insoluble sulfur produced in the second step is immersed in carbon disulfide for continuous extraction and stabilization, so th...

Embodiment 2

[0039] The method for preparing insoluble sulfur by capping the molecular chain of sulfur monomer quenching polymerization product, specifically includes the following steps:

[0040] In the first step, after the solid sulfur is melted, the temperature is raised to 120°C, and then gradually gasified to 580°C.

[0041] In the second step, the sulfur vapor vaporized in the first step is sprayed into the tank with a nozzle at a speed of 400Kg / hr, and the temperature is 15°C, the sulfur mass ratio is 15:1, and contains 0.02 parts by weight of elemental iodine and 0.03 parts by weight of iodine. Parts of potassium nitrate in carbon disulfide solution are atomized and contacted, and cooled; the formed pseudoplastic is powder, the particle size distribution is less than 80 mesh, and the content is 97%, and the intermediate contains 58% of insoluble sulfur.

[0042] In the third step, the insoluble sulfur produced in the second step is immersed in carbon disulfide for continuous extract...

Embodiment 3

[0046] The method for preparing insoluble sulfur by capping the molecular chain of sulfur monomer quenching polymerization product, specifically includes the following steps:

[0047] In the first step, after the solid sulfur is melted, the temperature is raised to 140°C, and gradually gasified to 635°C,

[0048] In the second step, the sulfur vapor vaporized in the first step is sprayed into the tank at a speed of 1200Kg / hr through the nozzle, and the temperature is 25°C, the sulfur mass ratio is 25:1, and contains 0.02 parts by weight of elemental iodine and 0.03 parts by weight of iodine. Parts of HClO in carbon tetrachloride solution are atomized and contacted, and cooled; the formed pseudoplastic is powder, the particle size distribution is less than 80 mesh, and the content is 93%, and the intermediate contains 58% of insoluble sulfur.

[0049] In the third step, the insoluble sulfur produced in the second step is immersed in carbon disulfide for continuous extraction an...

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Abstract

The invention discloses a method for preparing insoluble sulfur through blocking molecular chain of a quenching polymerization product of a sulfur monomer. The method specifically comprises the following steps: (1) melting and heating raw material sulfur into a flowing state and heating liquid-state sulfur for gradual gasification, so as to form sulfur steam; (2) spraying the sulfur steam obtained by gasification in step (1) into a pot with a spraying head, pressurizing quenching liquid to spray out atomized liquid drops, performing atomization contact on the atomized liquid drops and the sulfur steam to complete an addition reaction of two ends of the molecular chain and cooling, so as to obtain an intermediate containing the insoluble sulfur; (3) soaking the intermediate containing the insoluble sulfur obtained in step (2) into carbon disulfide for continuous extraction and stabilization; (4) transforming the materials into a dryer for drying; (5) charging extending oil specially used for rubber, so as to form an insoluble sulfur product. The sulfur steam is in full contact with the highly atomized quenching liquid, the insoluble sulfur is made into powder once, and the insoluble sulfur product is formed after extraction, drying, oil charging and secondary stabilization, therefore, the heat stability is improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemical industry, and particularly relates to a method for preparing insoluble sulfur by capping the molecular chain of a sulfur monomer quenching and cooling polymerization product. Background technique [0002] Polymeric sulfur is formed by the rapid cooling of high temperature sulfur gas and is the main component of insoluble sulfur. Polymeric sulfur usually has a molecular weight greater than 20,000. The solubility of polymerized sulfur in CS2 is extremely low. Since the polymerized sulfur usually encapsulates the raw material sulfur that is easily soluble in CS2 during the formation process, CS2 is usually used as the extractant in the production process of insoluble sulfur to extract the raw material sulfur. [0003] The raw material sulfur exists in the form of S8 at a lower temperature, that is, the eight sulfur atoms form a stable eight-membered ring. After heating up to a molten state of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/12
CPCC01B17/12C01P2004/61C01P2006/12C01P2006/37C01P2006/80
Inventor 尹进华
Owner QINGDAO UNIV OF SCI & TECH
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