CN101759150B - Method for drying hydrogen chloride gas - Google Patents
Method for drying hydrogen chloride gas Download PDFInfo
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- CN101759150B CN101759150B CN2010100113020A CN201010011302A CN101759150B CN 101759150 B CN101759150 B CN 101759150B CN 2010100113020 A CN2010100113020 A CN 2010100113020A CN 201010011302 A CN201010011302 A CN 201010011302A CN 101759150 B CN101759150 B CN 101759150B
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- hydrogen chloride
- chloride gas
- silicon tetrachloride
- spray column
- drying
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Abstract
The invention relates to a method for drying a hydrogen chloride gas, which comprises: allowing the hydrogen chloride gas containing water to rise from the bottom part of a drying spray tower along the inner cavity of the drying spray tower; spraying silicon tetrachloride in the inner cavity of the drying spray tower; performing the spray treatment of the hydrogen chloride gas; allowing the sprayed hydrogen chloride gas and the silicon tetrachloride mixed with the hydrogen chloride gas to enter a condenser from the top part of the drying spray tower to perform condensation treatment; and discharging the dried hydrogen chloride gas from the condenser. The silicon tetrachloride decomposes upon the contact with water to form the hydrogen chloride gas and silicon dioxide. The drying of the HCl by using the silicon tetrachloride has the advantages that: the generated HCl can be reused; the water content of the hydrogen chloride gas is reduced to below 50ppm; the conversion rate of silicon powder is improved; the production cost is reduced; the maximum temperature requirement by equipment for operation is 0 DEG C; the cold energy consumption is low; the equipment investment is small; the energy consumption is reduced; and the environmental pollution is relieved.
Description
Technical field
The present invention relates to the raw materials for production in a kind of trichlorosilane production, specifically, relate to the drying means of hydrogen chloride gas in the trichlorosilane production, belong to chemical technology field.
Background technology
Trichlorosilane is a colourless liquid, and is volatile, is prone to deliquescence.The main raw material of trichlorosilane production is industrial silicon and HCl, adopts silica flour and hydrogen chloride gas in fluidized-bed reactor, to generate, and meets the water decomposition reaction and produces hydrogen chloride gas.Belong to the one-level dangerous when wet, inflammable and explosive, it and oxygenant generation kickback are met naked light, highly burning are taken place when hot or explode.The optimal external condition of trichlorosilane production is a support with the chlor-alkali plant exactly, and the chlorine of existing direct conveying has cheap hydrogen again; But contain a large amount of moisture in the synthetic HCL gas, in case in the moisture entering system, will with the trichlorosilane generation silicon-dioxide that reacts; Stop up the equipment of next step production process, finally cause the transformation efficiency of silica flour to reduce, increase production cost; Therefore, the water cut in the control starting material hydrogenchloride is to improve transformation efficiency, the key that reduces production costs.
Silicon tetrachloride is the by product in the production process of trichlorosilane, utilizes narrow range at present, and relatively is difficult to handle, and has and meets the character that moisture promptly decomposes, and generates hydrogenchloride and silicon-dioxide with the water reaction, does not have other impurity.
Traditional technology is to reduce the moisture content of hydrogen chloride gas through the method for frozen cooling; Its technology be utilize-35 ℃ chilled brine with the HCL gas cooling to-17 ℃, just can the most moisture in the HCL gas be cooled off, thereby reach the purpose of dry HCL gas; But this arts demand consumes lot of energy; And equipment used need adopt graphite to process, and investment is big, and the water cut of handling post chlorization hydrogen is about 1000ppm; Water cut is still higher, can not tackle the problem at its root.
Summary of the invention
The problem that the present invention will solve is the deficiency to prior art, and a kind of drying means and equipment of hydrogen chloride gas is provided, and adopts this method can effectively reduce the water cut of hydrogen chloride gas and the production cost of trichlorosilane.
For overcoming the above problems, technical scheme of the present invention is following: a kind of drying means of hydrogen chloride gas is characterized in that: said drying means may further comprise the steps:
A, the hydrogen chloride gas that contains moisture enter into the bottom of dry spray column, and the inner chamber from the bottom along dry spray column is up;
B, spray silicon tetrachloride, hydrogen chloride gas is sprayed processing at the inner chamber of dry spray column;
C, the hydrogen chloride gas after spray is handled and get into condensing surface from the top of dry spray column with hydrogen chloride gas blended silicon tetrachloride carry out condensation process;
D, dried hydrogen chloride gas are discharged from condensing surface.
Further improvement as technique scheme:
Among the step a, the temperature of hydrogen chloride gas is 35 ℃-45 ℃.
Among the step b, be respectively equipped with spray header on bottom, middle part and the top of dry spray column, silicon tetrachloride through the bottom, the spray header on middle part and top sprays processing to hydrogen chloride gas.
Among the step c, condensed silicon tetrachloride liquid gets in the circulation tank.
The present invention adopts above technical scheme, compared with prior art, has the following advantages:
(1) utilize silicon tetrachloride to meet moisture and decompose, generate hydrogen chloride gas does not have other impurity with silicon-dioxide character, the use silicon tetrachloride carries out drying to HCL; The HCL that produces can utilize again; And silicon-dioxide can be discharged as solid, the water cut of hydrogen chloride gas is dropped to below the 50ppm, thereby improved the transformation efficiency of silica flour; Reduce production costs, also reduced the probability that equipment stops up in the postorder production process.
(2) as the sub product in the trichlorosilane production, the processing of silicon tetrachloride at present is difficulty relatively, and the present invention can make full use of the silicon tetrachloride that produces in the production, has solved silicon tetrachloride and has handled difficult problem.
(3) boiling point of silicon tetrachloride is 57.6 ℃, and the boiling point of hydrogenchloride is-85 ℃, differs bigger, and therefore, the silicon tetrachloride of in dry spray column, discharging with hydrogen chloride gas is easy to after condensation, separate with hydrogen chloride gas.
(4) among the present invention equipment move temperature required minimum be 0 ℃, compared with prior art, its consumption cold greatly reduces, and has reduced facility investment, the economy price ratio is high, has reduced the energy consumption of trichlorosilane production technique, has reduced environmental pollution simultaneously.
Below in conjunction with accompanying drawing and embodiment the present invention is described further:
Description of drawings
Accompanying drawing is the flowage structure synoptic diagram of drying means in the embodiment of the invention.
Among the figure,
The 1-pipeline, the dry spray column of 2-, 3-circulation tank, 4-recycle pump, 5-strainer, 6,7, the 8-spray header, 9-condensing surface, 10,11,12,13, the 14-pipeline.
Specific embodiment
Embodiment 1, a kind of drying means of hydrogen chloride gas, and the hydrogen chloride gas that contains moisture is from production plant come out to enter into through pipeline 1 bottom of dry spray column 2, and the charge flow rate of hydrogen chloride gas is 900Nm
3/ h, temperature is 35 ℃, pressure is 130kPaG; Water cut is 8000-10000ppm, and is up along the inner chamber of dry spray column 2 from the bottom, and silicon tetrachloride is stored in the circulation tank 3; Silicon tetrachloride is extracted out from circulation tank 3 by recycle pump 4 after strainer 5 filters, and pumps in the dry spray column 2; Spray processing successively from the spray header 6 that is arranged on dry spray column 2 bottoms, the spray header 7 at middle part and 8 pairs of hydrogen chloride gas of spray header on top, it is up along the inner chamber of dry spray column 2 that silicon tetrachloride is met the hydrogen chloride gas that produces after the water hydrolysis, and the silica solid of generation falls along the inner chamber of dry spray column 2; Discharge bottom at dry spray column 2, and dried hydrogen chloride gas gets into condensing surface 9 from the top of dry spray column 2, and hydrogen chloride gas is taken the part silicon tetrachloride to condensing surface 9 out of from dry spray column 2; 0 ℃ water of condensation gets into condensing surfaces 9 from pipeline 12, will carry out condensation with hydrogen chloride gas blended silicon tetrachloride after, come out from pipeline 11; Condensed silicon tetrachloride liquid is recovered in the circulation tank 3 along pipeline 10; The hydrogen chloride gas that comes out from condensing surface 9 enters into the production process of trichlorosilane again through pipeline 13, and the air outlet temperature of hydrogen chloride gas is 10 ℃, the collecting part hydrogen chloride gas; Through the test water cut is 49.2ppm, and the silicon tetrachloride in 14 pairs of circulation tanks 3 of pipeline replenishes.
Embodiment 2, a kind of drying means of hydrogen chloride gas, and the hydrogen chloride gas that contains moisture is from production plant come out to enter into through pipeline 1 bottom of dry spray column 2, and the charge flow rate of hydrogen chloride gas is 950Nm
3/ h, temperature is 40 ℃, pressure is 140kPaG; Water cut is 8000-10000ppm, and is up along the inner chamber of dry spray column 2 from the bottom, and silicon tetrachloride is stored in the circulation tank 3; Silicon tetrachloride is extracted out from circulation tank 3 by recycle pump 4 after strainer 5 filters, and pumps in the dry spray column 2; Spray successively from the spray header 6 that is arranged on dry spray column 2 bottoms, the spray header 7 at middle part and 8 pairs of hydrogen chloride gas of spray header on top, it is up along the inner chamber of dry spray column 2 that silicon tetrachloride is met the hydrogen chloride gas that produces after the water hydrolysis, and the silica solid of generation falls along the inner chamber of dry spray column 2; Discharge in the bottom of dry spray column 2, the hydrogen chloride gas that comes out from condensing surface 9 gets into condensing surface 9 from the top of dry spray column 2, and hydrogen chloride gas is taken the part silicon tetrachloride to condensing surface 9 out of from dry spray column 2; 0 ℃ water of condensation gets into condensing surfaces 9 from pipeline 12, will carry out condensation with hydrogen chloride gas blended silicon tetrachloride after, come out from pipeline 11; Condensed silicon tetrachloride liquid is recovered in the circulation tank 3 along pipeline 10; Dried hydrogen chloride gas enters into the production process of trichlorosilane again through pipeline 13, and the air outlet temperature of hydrogen chloride gas is 13 ℃, the collecting part hydrogen chloride gas; Through the test water cut is 48.5ppm, and the silicon tetrachloride in 14 pairs of circulation tanks 3 of pipeline replenishes.
Embodiment 3, a kind of drying means of hydrogen chloride gas, and the hydrogen chloride gas that contains moisture is from production plant come out to enter into through pipeline 1 bottom of dry spray column 2, and the charge flow rate of hydrogen chloride gas is 1000Nm
3/ h, temperature is 45 ℃, pressure is 150kPaG; Water cut is 8000-10000ppm, and is up along the inner chamber of dry spray column 2 from the bottom, and silicon tetrachloride is stored in the circulation tank 3; Silicon tetrachloride is extracted out from circulation tank 3 by recycle pump 4 after strainer 5 filters, and pumps in the dry spray column 2; Spray successively from the spray header 6 that is arranged on dry spray column 2 bottoms, the spray header 7 at middle part and 8 pairs of hydrogen chloride gas of spray header on top, it is up along the inner chamber of dry spray column 2 that silicon tetrachloride is met the hydrogen chloride gas that produces after the water hydrolysis, and the silica solid of generation falls along the inner chamber of dry spray column 2; Discharge bottom at dry spray column 2, and dried hydrogen chloride gas gets into condensing surface 9 from the top of dry spray column 2, and hydrogen chloride gas is taken the part silicon tetrachloride to condensing surface 9 out of from dry spray column 2; 0 ℃ water of condensation gets into condensing surfaces 9 from pipeline 12, will carry out condensation with hydrogen chloride gas blended silicon tetrachloride after, come out from pipeline 11; Condensed silicon tetrachloride liquid is recovered in the circulation tank 3 along pipeline 10; The hydrogen chloride gas that comes out from condensing surface 9 enters into the production process of trichlorosilane again through pipeline 13, and the air outlet temperature of hydrogen chloride gas is 15 ℃, the collecting part hydrogen chloride gas; Through the test water cut is 48.8ppm, and the silicon tetrachloride in 14 pairs of circulation tanks 3 of pipeline replenishes.
Claims (1)
1. the drying means of a hydrogen chloride gas, it is characterized in that: said drying means may further comprise the steps:
A, the hydrogen chloride gas that contains moisture enter into the bottom of dry spray column (2), and up along the inner chamber of dry spray column (2) from the bottom, the temperature of hydrogen chloride gas is 35 ℃-45 ℃;
B, spray silicon tetrachloride, be respectively equipped with spray header on bottom, middle part and the top of dry spray column (2) at the inner chamber of dry spray column (2), silicon tetrachloride through the bottom, the spray header on middle part and top sprays processing to hydrogen chloride gas;
C, the hydrogen chloride gas after spray is handled and get into condensing surface (9) from the top of dry spray column (2) with hydrogen chloride gas blended silicon tetrachloride carry out condensation process;
D, dried hydrogen chloride gas are discharged from condensing surface (9), and condensed silicon tetrachloride liquid gets in the circulation tank (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100113020A CN101759150B (en) | 2010-01-04 | 2010-01-04 | Method for drying hydrogen chloride gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100113020A CN101759150B (en) | 2010-01-04 | 2010-01-04 | Method for drying hydrogen chloride gas |
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| CN101759150A CN101759150A (en) | 2010-06-30 |
| CN101759150B true CN101759150B (en) | 2012-07-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010100113020A Expired - Fee Related CN101759150B (en) | 2010-01-04 | 2010-01-04 | Method for drying hydrogen chloride gas |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905888A (en) * | 2010-08-23 | 2010-12-08 | 湖北新蓝天新材料股份有限公司 | Method for producing trichlorosilane |
| CN102153051A (en) * | 2011-05-19 | 2011-08-17 | 河北邢矿硅业科技有限公司 | Method for removing moisture in hydrogen chloride gas |
| CN102249244B (en) * | 2011-06-15 | 2013-05-08 | 四川瑞能硅材料有限公司 | HCl dehydration and purification method suitable for synthesis of trichlorosilane |
| CN102417163A (en) * | 2011-07-28 | 2012-04-18 | 四川瑞能硅材料有限公司 | Improved Siemens method-HCL gas dehydration purifying method |
| CN107746040B (en) * | 2017-10-17 | 2021-04-13 | 山东新龙科技股份有限公司 | Process and equipment for refining hydrogen chloride by using byproduct gas from production of trichloroethylene |
| CN111137862A (en) * | 2019-12-25 | 2020-05-12 | 中船重工（邯郸）派瑞特种气体有限公司 | Hydrogen chloride raw material gas moisture removal device and moisture removal method |
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Owner name: SHANDONG XINLONG TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: SHANDONG XINLONG SILICAS INDUSTRY SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20140211 |
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Effective date of registration: 20140211 Address after: 262709 New Dragon Industrial Zone, Shouguang City, Shandong Patentee after: Shandong Xinlong Technology Co., Ltd. Address before: 262700 Shandong Province, Shouguang City, Wang Xinlong Industrial Park Shandong Xinlong high silicon industry Co. Ltd. Patentee before: Shandong Xinlong Silicas Industry Science and Technology Co., Ltd. |
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