CN100434431C - Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas - Google Patents
Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas Download PDFInfo
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- CN100434431C CN100434431C CNB031000339A CN03100033A CN100434431C CN 100434431 C CN100434431 C CN 100434431C CN B031000339 A CNB031000339 A CN B031000339A CN 03100033 A CN03100033 A CN 03100033A CN 100434431 C CN100434431 C CN 100434431C
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Abstract
The present invention discloses a wet dust removal technology of an organochlorosilane gas. The technology of the present invention comprises the following steps: a synthesis gas from a two stage cyclone separator enters a washing tower through the bottom of the washing tower, a material liquid discharged from a tower kettle enters a flash tank, the flashed gas enters a flash condenser to be condensed, incondensable gas is emptied after being washed in a water washing tower, the condensed liquid enters a recovery liquid receiving groove, and slag is discharged in a waste slag groove. Gas on the tower top enters a precooler on the top of the washing tower and deep cooled through a condenser on the top of the washing tower, incondensable gas enters a methyl chloride buffer tank, and the condensed liquid enters a thick monomer intermediate tank; part of the discharged material flows back into the tower, and part of the discharged material is processed in a thick monomer tower.
Description
Technical field
Continuous wet dedusting of using inorganic chlorosilane gas disclosed by the invention and the height separating technology that boils has characteristics such as efficiency of dust collection height, labour intensity is low, loss of material is little.
Background technology
Both at home and abroad in patent and the document, few in the past to the report of using inorganic chlorosilane gas wet dedusting Processes and apparatus, Chinese patent provide wet dedusting in a kind of synthesizing methyl-chloro-silane washings utilize method.Its process is with the industrial ethyl esterification of 0: 1 to 1: 3 washings of solid-to-liquid ratio, the ethanol consumption is 1.0～1.3 times of cl contenies in the washings, or use 40% aqueous sodium hydroxide solution alkali molten again, and make waterproofing agent of organosilicon, can be used for the WATER REPELLENT of buildings or material of construction.This patent is only mentioned the method for utilizing of washings after the wet dedusting, and using inorganic chlorosilane gas wet dedusting Processes and apparatus is not mentioned.
Summary of the invention
The invention describes a kind of using inorganic chlorosilane gas wet dedusting technology and the height separating technology that boils.
High-temperature synthesis gas from secondary cyclone, enter washing tower from wash tower bottoms, control tower top pressure and washing reflux ratio, after the washings washing, temperature is reduced to 50-90 ℃, to tower still revaporizer, the revaporizer heat-conducting oil heating is controlled the revaporizer gas phase temperature to liquid-solid body impurity such as washings and silica flour from the overflow of tower still.The revaporizer liquid level enters flash tank by its two formula on-off control in bottom with the methyl chlorosilane high boiling material of dust-laden, and the gas after the flash distillation enters flash condenser and carries out condensation, and noncondensable gas is by water wash column washing back emptying, and phlegma enters and reclaims the liquid groove.Residue after the flash distillation is put into the waste residue groove.
Overhead gas enters washing tower cat head pre-cooler, and gas phase enters the washing tower overhead condenser and carries out condensation, and-15 ℃ of aqueous glycol solutions are adopted in condensation.Condensed non-condensable gas dechlorination methane surge tank.The phlegma of washing tower cat head pre-cooler and washing tower condenser enters the crude monomer tundish, getting back to washing tower by the washing tower reflux pump refluxes, with the temperature that reduces synthetic gas and remove impurity in the methyl chlorosilane, part discharging simultaneously send the crude monomer tower to handle.
The present invention has the following advantages:
The present invention adopts continuous wet dedusting technology to substitute traditional dry dedusting technology.Be that using inorganic chlorosilane gas enters from wash tower bottoms, enter cat head pre-cooler and condenser more successively, noncondensable gas is sent into surge tank, the phlegma partial reflux, and part enters next system.The slurries that reboiler is discharged enter flash tank, and the gas after the flash distillation enters flash condenser and carries out condensation, and phlegma is sent into the height storage tank that boils.This technology can thoroughly be removed the dust in the methyl chlorosilane gas and reduce to methyl chlorosilane gas temperature required.
Following processing condition all are suitable to the present invention:
6. the slurry solid content of vaporizer is 20-40wt%.
7. flash tank discharge slurry solid content is 30-70wt%.
8. the scrubber overhead temperature is 5090 ℃ (best for 60-80 ℃).
9. the washing tower tower top pressure is 0.20.4Mpa.
10. the washing tower reflux ratio is 0.5-2 (the best 0.9-1.5 of being).
Embodiment:
High-temperature synthesis gas from secondary cyclone, enter washing tower from wash tower bottoms, the control tower top pressure is 0.3MPa, reflux when 60 ℃ of tower top temperatures of washing tower, after the washings washing, temperature is reduced to 70 ℃, and liquid-solid body impurity such as washings and silica flour are from the overflow of tower still to tower still revaporizer, the revaporizer heat-conducting oil heating, control revaporizer gas phase temperature is 220 ℃.The revaporizer liquid level is by its two formula on-off control in bottom, the methyl chlorosilane height of the dust-laden of solid content 30% boiled enter flash tank, gas after the flash distillation enters flash condenser and carries out condensation, and noncondensable gas is by water wash column washing back emptying, and phlegma enters and reclaims the liquid groove.Residue after the flash distillation (solid content is 40%) enters the waste residue groove.
Overhead gas enters washing tower cat head pre-cooler, and gas phase enters the washing tower overhead condenser and carries out condensation, and-15 ℃ of aqueous glycol solutions are adopted in condensation, and control scrubber overhead temperature is 70 ℃.Condensed non-condensable gas dechlorination methane surge tank.The phlegma of scrubber overhead pre-cooler and washing tower condenser enters the crude monomer tundish, gets back to washing tower by the washing tower reflux pump and refluxes, and part discharging simultaneously send the crude monomer tower to handle.
Detailed process flow is seen Figure of description.
Claims (1)
1, the wet dedusting of organochlorosilane synthetic gas and the height separating technology that boils, comprise high-temperature synthesis gas from secondary cyclone, enter washing tower from wash tower bottoms, control tower top pressure and washing tower reflux ratio, after the washings washing, liquid-solid body impurity such as washings and silica flour from the overflow of tower still to tower still revaporizer, the revaporizer liquid level is by its two formula on-off control in bottom, still liquid is entered flash tank, gas after the flash distillation enters flash condenser and carries out condensation, phlegma enters and reclaims the liquid groove, residue after the flash distillation enters the waste residue groove, overhead gas enters the washing tower overhead condenser and carries out condensation, condensed non-condensable gas dechlorination methane surge tank, phlegma enters the crude monomer tundish, getting back to washing tower by the washing tower reflux pump refluxes, part discharging simultaneously send the crude monomer tower to handle, the slurry solid content that it is characterized in that revaporizer is 20-40wt%, it is 30-70wt% that flash tank is discharged slurry solid content, the scrubber overhead temperature is 50-90 ℃, the washing tower tower top pressure is 0.2-0.4Mpa, and the washing tower reflux ratio is 0.5-2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031000339A CN100434431C (en) | 2003-01-07 | 2003-01-07 | Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031000339A CN100434431C (en) | 2003-01-07 | 2003-01-07 | Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1438226A CN1438226A (en) | 2003-08-27 |
| CN100434431C true CN100434431C (en) | 2008-11-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031000339A Expired - Fee Related CN100434431C (en) | 2003-01-07 | 2003-01-07 | Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417923B (en) * | 2008-12-01 | 2011-08-17 | 山东东岳有机硅材料有限公司 | Methyl chloride recovery and refining method |
Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337974B (en) * | 2008-08-08 | 2011-03-16 | 北京石油化工设计院有限公司 | Energy-conserving process for washing and dedusting by methyl monomer synthesis gas |
| CN101434510B (en) * | 2008-12-19 | 2011-09-28 | 山东东岳有机硅材料有限公司 | Method and apparatus for recovering methyl chloride in organosilicon monomer synthesis |
| CN101440102B (en) * | 2008-12-19 | 2011-07-20 | 山东东岳有机硅材料有限公司 | Method for processing methyl monomer synthesized washing slurry |
| WO2011094938A1 (en) * | 2010-02-04 | 2011-08-11 | 南京工业大学 | Dry dust removal method in organic chlorosilane production |
| CN101792460B (en) * | 2010-02-04 | 2012-06-27 | 南京工业大学 | Dry dedusting method for organochlorosilane production |
| CN102372271B (en) * | 2011-08-17 | 2014-06-11 | 乐山乐电天威硅业科技有限责任公司 | Recovery method of waste chlorsilane in polysilicon produced through modified Simens Method |
| CN102515183B (en) * | 2011-12-08 | 2013-04-03 | 飞潮（无锡）过滤技术有限公司 | Method and device for treating chlorosilane liquid produced in polysilicon production |
| CN102908795B (en) * | 2012-09-17 | 2015-08-05 | 中国恩菲工程技术有限公司 | A kind of processing method of technique of trichlorosilane synthetic tail gas and system |
| CN104415560A (en) * | 2013-08-24 | 2015-03-18 | 内蒙古盾安光伏科技有限公司 | Polysilicon cold hydrogenation raffinate recovery system |
| CN105037414A (en) * | 2015-07-29 | 2015-11-11 | 湖北兴瑞化工有限公司 | Method and device for recovering efficient high-boiling substance from organic silicon residue slurry |
| CN105597462A (en) * | 2016-03-16 | 2016-05-25 | 山东东岳有机硅材料有限公司 | Treatment process for dust-containing tail gas in synthesis and emptying of methyl chlorosilane |
| CN106012941B (en) * | 2016-07-08 | 2017-08-11 | 黄河科技学院 | Construction building site rail mounted sized spray dust-suppression system |
| CN109134527B (en) * | 2018-09-07 | 2020-11-24 | 江西蓝星星火有机硅有限公司 | Washing tower system and application thereof in separation of methyl chlorosilane monomers |
| CN110314400B (en) * | 2019-07-30 | 2023-12-26 | 合盛硅业（泸州）有限公司 | Slurry and slag discharging device and method for organic silicon production |
| CN110743184B (en) * | 2019-11-01 | 2022-04-19 | 新疆东方希望新能源有限公司 | Residual removing processing system and method |
| CN113861232B (en) * | 2021-10-08 | 2024-05-28 | 华陆工程科技有限责任公司 | Improved method and device for energy conservation and quality improvement of organosilicon production system |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102886A (en) * | 1985-04-01 | 1986-09-17 | 吉林化学工业公司研究院 | The utilization of the cleaning solution of wet dedusting in the synthesizing methyl-chloro-silane |
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2003
- 2003-01-07 CN CNB031000339A patent/CN100434431C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85102886A (en) * | 1985-04-01 | 1986-09-17 | 吉林化学工业公司研究院 | The utilization of the cleaning solution of wet dedusting in the synthesizing methyl-chloro-silane |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101417923B (en) * | 2008-12-01 | 2011-08-17 | 山东东岳有机硅材料有限公司 | Methyl chloride recovery and refining method |
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| CN1438226A (en) | 2003-08-27 |
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