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Gasification quenching technology of insoluble sulfur

A sulfur and quenching technology, applied in the direction of sulfur preparation/purification, etc., can solve the problems of wide particle size distribution of semi-finished insoluble sulfur products, no improvement in the contact mode of quenching medium, and difficulty in controlling the thermal stability and dispersion of finished products. , to achieve the effect of fine product particles, low production cost, and sufficient quenching

Active Publication Date: 2015-03-11
SHANDONG YANGGU HUATAI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process does not improve or optimize the quenching process, and still uses the traditional process method
[0005] Chinese patent document CN102398896B provides a production process of insoluble sulfur for rubber. Although the process adopts the step of gasification quenching, there is no improvement in the selection of quenching medium and the contact mode in the quenching process. Quenching liquid for direct impact quenching
[0006] It is known from the prior art that because the polymerized sulfur is impact quenched in a liquid state, the insoluble sulfur product obtained has technical problems such as wide particle size distribution of the semi-finished product, long extraction process, difficult control of the thermal stability and dispersibility of the finished product, etc.

Method used

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  • Gasification quenching technology of insoluble sulfur

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Experimental program
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Effect test

Embodiment 1

[0027] Add the prepared 20 ℃, 100L carbon disulfide quenching liquid into a vertical reaction tank with a jacket (heat exchange device) with a volume of 300 L, and use a circulation pump to extract the carbon disulfide quenching liquid from the bottom of the vertical reaction tank and transport it to The spraying device in the upper part of the reaction tank is used for spraying, and a liquid curtain of circulating spray is formed in the vertical reaction tank. The liquid curtain is in the shape of a shower spray. The flow rate of the circulating pump is controlled at 1500L / h, and the pressure in the reaction tank is maintained at 0.01 MPa.

[0028] The liquid sulfur heated to 550°C-580°C in the heating device with an internal pressure of 0.6Mpa is passed into the upper liquid curtain of the vertical reaction tank at a rate of 1.05kg / min, and the circulating water volume in the jacket of the vertical reaction tank is controlled. Keep the temperature of the material in the tank...

Embodiment 2

[0032] The gasification and quenching process of insoluble sulfur described in this embodiment is as described in Example 1, the difference is that the liquid sulfur is heated to 600°C-610°C in a heating device with an internal pressure of 1Mpa and At a speed of 1.05kg / min, it is passed into the liquid curtain at the upper part of the vertical reaction tank whose pressure is maintained at 0.1Mpa and the temperature is 60°C; the temperature of the solid-liquid two-phase material obtained at last is 70°C, and the mass concentration of the solid phase is 35%. , the solid-liquid two-phase material in the lower part of the vertical reaction tank is sucked and washed with 100kg carbon disulfide, and then sent to a vacuum drying oven for sufficient drying to obtain 25.8kg insoluble sulfur powder with a yield of 51.6%. The detection indexes are as follows: thermal stability at 120° C. for 15 minutes is 56.1%, average particle size is 34 microns, and purity is 96.3%.

Embodiment 3

[0034] The gasification and quenching process of insoluble sulfur described in this embodiment is as described in Example 1, the difference is that the liquid sulfur is heated to 620°C-630°C in a heating device with an internal pressure of 1Mpa and Pass into the liquid curtain on the upper part of the vertical reaction tank by the speed of 0.9kg / min; The solid-liquid two-phase material was suction-filtered and washed with 100 kg of carbon disulfide, then sent to a vacuum drying oven for sufficient drying to obtain 26.3 kg of insoluble sulfur powder with a yield of 52.6%. The detection indexes are as follows: thermal stability at 120° C. for 15 minutes is 57.3%, average particle diameter is 29 microns, and purity is 97.1%.

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Abstract

The invention relates to a gasification quenching technology of insoluble sulfur. In the provided technology, the liquid sulfur is heated to an over-heated state, then the liquid sulfur in an over-heated state is sprayed into a liquid screen made of cooling medium, which is sprayed cyclically; under the great pressure difference, the over-heated liquid sulfur is converted into dispersed gas and moist, the sulfur gas and moist are fully quenched and absorbed by the cooling medium, and then the cooling medium containing the sulfur is transferred to the lower part of a reaction tank to carry out solidification and extraction in a liquid cooling medium environment so as to obtain the insoluble sulfur. The cooling medium is cyclically sprayed to form a liquid screen, while in the conventional method the cooling medium is directly added into the liquid sulfur, moreover, the contact surface between the sulfur (moist and gas) and the cooling medium is enlarged through the liquid screen, the quenching on the sulfur (moist and gas) can be more complete and fine, and the rough treatment in the conventional quenching process is avoided. The insoluble sulfur product prepared by the provided method has the advantages of fine particles, high purity, and good dispersibility, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a gasification and quenching process of insoluble sulfur, in particular to a production process for converting sulfur into insoluble sulfur by quenching in a carbon disulfide environment, and belongs to the technical field of fine chemicals. Background technique [0002] Insoluble sulfur is obtained by thermal polymerization of ordinary sulfur and is insoluble in carbon disulfide. As a high-grade accelerator and vulcanization crosslinking agent in the rubber industry, it has the functions of not blooming and improving the adhesion between layers of multi-layer rubber products. It has the advantages of high bonding strength, effective reduction of scorch phenomenon during storage of rubber materials, etc. It is an essential and important raw material in tire production, especially in the production of automotive all-steel radial tires. [0003] Usually, insoluble sulfur is produced by heating molten liquid sulfur to a certain t...

Claims

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Application Information

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IPC IPC(8): C01B17/12
CPCC01B17/12
Inventor 杜孟成王维民魏承磊
Owner SHANDONG YANGGU HUATAI CHEM
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