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Method of producing high-pure sulfur

A production method and high-purity sulfur technology, applied in the preparation/purification of sulfur, etc., can solve problems such as poor effect, and achieve the effects of high purity, good product quality, and easy industrial production.

Inactive Publication Date: 2008-02-20
四川鑫龙碲业科技开发有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process currently used at home and abroad is the elemental distillation method, but the effect is poor

Method used

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  • Method of producing high-pure sulfur

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 3.0 kilograms of 99wt% sulfur into the crucible 4, then put the crucible with 99wt% sulfur into the quartz tube 6, put the quartz tube into the heating furnace 1 for vacuum sublimation, and set the insulation layer 2 and the heating wire in the heating furnace 3. Crucible 4, furnace lining 5, quartz tube 6 and vacuum gland 7. The inclination angle α installed in the heating furnace is 30°. One end of the quartz tube is sealed with vacuum gland 7, and the vacuum gland is provided with a vacuum port, which is evacuated to 1×10 -3 Pa, turn on the heating system of the vacuum sublimation heating furnace, wait for the temperature of the heating furnace to rise to 135 ° C, carry out vacuum sublimation and purification for 4.5 hours, then close the vacuum and heating system, cool and discharge, and obtain 2.3 kg of 5N sulfur product, the yield is 78% .

Embodiment 2

[0017] Put 3.5 kilograms of 99wt% sulfur into the crucible 4, then put the crucible with 99wt% sulfur into the quartz tube 6, put the quartz tube into the heating furnace 1 for vacuum sublimation, and set the insulation layer 2 and the heating wire in the heating furnace 3. Crucible 4, furnace lining 5, quartz tube 6 and vacuum gland 7. The inclination angle α installed in the heating furnace is 40°. One end of the quartz tube is sealed with a vacuum gland 7, and a vacuum port is provided on the vacuum gland to evacuate to 5×10 -3 Pa, turn on the heating system of the vacuum sublimation heating furnace, wait for the temperature of the heating furnace to rise to 140 ° C, carry out vacuum sublimation and purification for 4 hours, then turn off the vacuum and heating system, cool and discharge, and obtain 2.4 kg of 5N sulfur product, with a yield of 75%.

Embodiment 3

[0019] Put 4.0 kilograms of 99wt% sulfur into the crucible 4, then put the crucible with 99wt% sulfur into the quartz tube 6, put the quartz tube into the heating furnace 1 for vacuum sublimation, and set the insulation layer 2 and the heating wire in the heating furnace 3. Crucible 4, furnace lining 5, quartz tube 6 and vacuum gland 7. The inclination angle α installed in the heating furnace is 45°. One end of the quartz tube is sealed with a vacuum gland 7, and a vacuum port is provided on the vacuum gland to evacuate to 9×10 -3 Pa, turn on the heating system of the vacuum sublimation heating furnace, wait for the temperature of the heating furnace to rise to 145 ° C, carry out vacuum sublimation purification for 3.5 hours, then turn off the vacuum and heating system, cool and discharge, and obtain 3.0 kg of 5N sulfur product, the yield is 76% .

[0020] Table 15N impurity content of high-purity sulfur (in ppm)

[0021] Impurities

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Abstract

The invention provides a producing method of high pure sulfur, which is characterized in filling 3 to 4 weight parts of 99 wt percent sulfur into a pot(4), then putting the pot with 99 wt percent sulfur into a quartz tube(6) which is put into a vacuum sublimation heating furnace(1). Wherein, the heating furnace is internally provided with an insulation layer(2), a heating wire(3), a pot(4), a furnace lining(5), a quartz tube(6) and a vacuum pressure cover(7), whose mounting obliquity Alpha is 30 to 45 degrees; moreover, one end of the quartz tube is sealed with the vacuum pressure cover(7) which is provided with an extraction vacuum hole; once the vacuum is extracted to 1 multiplies by 10-3 to 9 multiplies by 10-3Pa, the heating system of the vacuum sublimation heating furnace is opened, after that, waiting till the temperature of the heating furnace is up to 135 to 145 DEG C, the vacuum sublimation purifying is performed for 3.5 to 4.5 hours; after that, the vacuum and heating system is closed for cooling and discharging, thus, obtaining 2.3 to 3.0 weight parts of 5N sulfur product and having a yield of 75 to 78 percent.

Description

technical field [0001] The invention relates to a production method of high-purity sulfur, which belongs to the field of high-purity sulfur preparation. Background technique [0002] High passive sulfur above 5N is mainly used in chalcogenide compound semiconductors, new generation light sources, photoconductive materials, imaging target surface materials (Sb 2 S 3 ) and photodetection materials (Sb 4 o 2 S 4 )field. With the rapid development of the optoelectronic industry, the demand for high-purity sulfur in domestic and foreign markets is increasing rapidly, but there are very few units engaged in the production and research of high-purity sulfur. Therefore, the research and development of high-purity sulfur has been included in the national science and technology support project. The production process currently adopted at home and abroad is the elemental distillation method, but the effect is poor. Contents of the invention [0003] The purpose of the present ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/02
Inventor 侯仁义
Owner 四川鑫龙碲业科技开发有限责任公司
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