CN101704524A - Production device and method of high purity trichlorosilane by using heat pump distillation - Google Patents

Production device and method of high purity trichlorosilane by using heat pump distillation Download PDF

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Publication number
CN101704524A
CN101704524A CN200910228635A CN200910228635A CN101704524A CN 101704524 A CN101704524 A CN 101704524A CN 200910228635 A CN200910228635 A CN 200910228635A CN 200910228635 A CN200910228635 A CN 200910228635A CN 101704524 A CN101704524 A CN 101704524A
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column
weight
lightness
condenser
tower
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CN200910228635A
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Chinese (zh)
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CN101704524B (en
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黄国强
王红星
李鑫钢
张瑞玲
张敏革
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天津大学
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Abstract

The invention relates to a production device and a method of high purity trichlorosilane by using heat pump distillation. Trichlorosilane raw materials enter a de-heavy fractionator to eliminate heavy components after light component elimination through a light component eliminating tower, thereby obtaining high purity trichlorosilane. On the basis, the light component eliminating tower and the de-heavy fractionator both adopt a heat pump distillation process. Cooling medium in a condenser absorbs heat after exchanging the heat with materials on the top of the tower and is evaporated into gas, the gas enters a reboiler as tower reactor heat source reactor liquid after pressure and temperature enhancement through compression, and the gas is condensed into liquid. The liquid returns to the condenser after reduction of expenditure and pressure so as to finish a cycle. Therefore, the heat at the low temperature part of the tower top is transferred to the high temperature part of a tower reactor through the cooling medium. The invention has the advantages that by adopting the heat pump distillation process, the energy consumption can be greatly lowered, and the annual economic benefit is greatly enhanced.

Description

High purity trichlorosilane by using heat pump distillation production equipment and method

Technical field

The present invention relates to the energy-conservation separation technology field of high-purity trichlorosilane, specifically is high purity trichlorosilane by using heat pump distillation production equipment and method.

Background technology

Polysilicon is the basic raw material of solar energy industry and semiconductor industry, is China's electronics and information industry and the necessary strategic materials of photovoltaic industry development.

The improvement Siemens Method is the main production method of the existing polysilicon of present China, can the compatible electronic level and the production of solar-grade polysilicon, comprise primary processes such as trichlorosilane is synthetic, trichlorosilane is purified, trichlorosilane reduction, reduction tail gas dry process rectifying recovery, hydrogenation of silicon tetrachloride, mainly have problems such as energy consumption height, potentially contaminated be serious.In this process, except that the trichlorosilane reduction, other process all relates to rectifying, and required distillation system has high reflux ratio and high theoretical stage feature, requires foreign matter contents such as B, P at the PPT order of magnitude, is highly energy-consuming, the high pollution process of generally acknowledging.At present, there are the significance difference distance in used distillation technology and developed country in the domestic production of polysilicon, have become one of major technique bottleneck of restriction China high quality polycrystalline silicon material production, are badly in need of technological breakthrough.

Heat pump distillation has been widely used in the various Chemical Manufacture as a kind of power-saving technology that can effectively improve rectified heat efficient.As at ethylbenzene-vinylbenzene, propylene-propane, Trimethylmethane-normal butane, systems such as ethane-ethylene must separate with alcohol production in, exist the example that successfully uses heat pump techniques in a large number, in recent years, along with polysilicon becomes the strategic industry that country first develops gradually, trichlorosilane isolation technique in the production of polysilicon technology is improved particularly difficulty, at present, this field does not still have the introduction of heat pump distillation technology, in view of heat pump distillation and technology can greatly reduce the production process energy consumption, obtain distinct economic, introduce heat pump techniques and have great advantage to cutting down the consumption of energy in the trichlorosilane sepn process, technical feasibility is higher.

Summary of the invention

Purpose of the present invention provides a kind of high purity trichlorosilane by using heat pump distillation separation method and device that cuts down the consumption of energy.It adopts two regular packed tower serial process, all adopts atmospheric operation.The heat-pump rectifying process that adopts it is advantageous that the tower working pressure is low, and unit consumption of energy is low, and production cost reduces greatly, and is simple in structure, safe and reliable.

Technology of the present invention is as follows:

A kind of high purity trichlorosilane by using heat pump distillation production equipment comprises lightness-removing column (1), lightness-removing column reboiler (4), condenser of light component removal column (3), lightness-removing column surge tank (7), lightness-removing column compressor (9), lightness-removing column dropping valve (18), heat pump (14), weight-removing column (2), weight-removing column condenser (5), weight-removing column surge tank (8), weight-removing column compressor (10), weight-removing column reboiler (6), weight-removing column dropping valve (24); Opening for feed is established at lightness-removing column (1) middle part, pipeline of lightness-removing column bottoms stream and the bottom of returning lightness-removing column (1) after lightness-removing column reboiler (4) is connected, another pipeline links to each other with the middle part of weight-removing column through pump (14), lightness-removing column (1) overhead stream links to each other with lightness-removing column surge tank (7) behind condenser of light component removal column (3), and lightness-removing column surge tank (7) outlet at bottom is provided with feed back and material extraction; Condenser of light component removal column (3) one ends link to each other with lightness-removing column reboiler (4) through lightness-removing column compressor (9) by pipeline, lightness-removing column reboiler (4) the other end links to each other with condenser of light component removal column (3) one ends through lightness-removing column dropping valve (18), forms the lightness-removing column heat pump circulating system; Weight-removing column (2) tower base stream and the bottom of returning weight-removing column (2) after weight-removing column reboiler (6) is connected, weight-removing column (2) overhead stream links to each other with weight-removing column surge tank (8) behind weight-removing column condenser (5), and weight-removing column surge tank (8) outlet at bottom is provided with feed back and material extraction; Weight-removing column condenser (5) one ends link to each other with weight-removing column reboiler (6) through weight-removing column compressor (10) by pipeline, weight-removing column reboiler (6) the other end links to each other with weight-removing column condenser (5) one ends through weight-removing column dropping valve (24), forms the weight-removing column heat pump circulating system.

Wherein heat pump adopts the enclosed heat pump.The condenser condenses medium adopts heat pump cycle working medium.The reboiler heating medium adopts heat pump cycle working medium.

A kind of high purity trichlorosilane by using heat pump distillation production method: trichlorosilane stock liquid (11) enters the middle part of lightness-removing column (1), returns lightness-removing column (1) through trichlorosilane solution (a 12) part at the bottom of the tower after taking off gently through lightness-removing column reboiler (4); Another part is squeezed into weight-removing column (2) by pump (14) and is taken off heavily; Lightness-removing column overhead gas phase materials (13) main component is dichloro-dihydro silicon and micro-light impurity, after condenser of light component removal column (3) cooling, enter lightness-removing column surge tank (7), return lightness-removing column (1), a part of extraction from the effusive material part of lightness-removing column surge tank (7); Weight-removing column cat head gas-phase product (15) enters weight-removing column surge tank (8) behind weight-removing column condenser (5), be high-purity trichlorosilane from weight-removing column surge tank (8) material that comes out, and wherein a part is returned weight-removing column (2), and a part is as the product extraction.

The heat pump cycle feature of lightness-removing column (1) is: the heat-eliminating medium (20) in the condenser of light component removal column (3) is lightness-removing column gas (21) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of lightness-removing column gas (21) and the temperature, enter lightness-removing column reboiler (4) as tower still thermal source still liquid, and itself condense into lightness-removing column liquid (17), lightness-removing column liquid (17) returns condenser of light component removal column (3) behind expenditure and pressure, finish a circulation; The heat pump cycle feature of weight-removing column (2) is: the heat-eliminating medium (22) in the weight-removing column condenser (5) is weight-removing column gas (23) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of weight-removing column gas (23) and the temperature, enter weight-removing column reboiler (6) as tower still thermal source still liquid, and itself condense into weight-removing column liquid (19), weight-removing column liquid (19) returns weight-removing column condenser (5) behind expenditure and pressure, finish a circulation.

The lightness-removing column reflux ratio is 20-50, and the weight-removing column reflux ratio is 3-10.Lightness-removing column pressure is 300KPa, and tower top temperature is controlled at 60~70 ℃, and the temperature difference is in 10 degree at the bottom of the cat head tower.Weight-removing column pressure is 600KPa, and tower top temperature is controlled at 80~90 ℃, and the temperature difference is controlled in 10 degree at the bottom of the cat head tower.

The product that slightly heats up in a steamer workshop section mainly contains trichlorosilane, dichloro-dihydro silicon, silicon tetrachloride and trace impurity, enter lightness-removing column and isolate dichloro-dihydro silicon and micro-light impurity by cat head, the bottoms material enters weight-removing column and isolates high-purity trichlorosilane product by cat head, and the bottoms material enters residual liquid tank.Because high-purity trichlorosilane product requirement is very high, electronic-grade need reach more than 99.9999999%, so lightness-removing column and weight-removing column all need big reflux ratio operation, the lightness-removing column reflux ratio is 20-50, weight-removing column reflux ratio 3-30, thereby power consumption is very big.Heat-pump rectifying process is applicable to that relatively rectification temperature is low, the rectifying tower that has a narrow range of temperature at the bottom of the cat head tower.

The present invention relates to high purity trichlorosilane by using heat pump distillation production equipment and method.Thereby enter weight-removing column again after the trichlorosilane stock liquid takes off gently through lightness-removing column and take off heavy high-purity trichlorosilane that obtains.Dehydrogenation tower and weight-removing column all adopt heat-pump rectifying process on this basis.Heat-eliminating medium in the condenser and cat head end material heat exchange post-absorption heat of vaporization are gas, after compressed pressurize of gas and the temperature, enter reboiler as tower still thermal source still liquid, and itself condense into liquid.Liquid returns condenser behind expenditure and pressure, finish a circulation.So the heat at cat head low temperature place is delivered to tower still high temperature place by heat-eliminating medium.Advantage of the present invention is to adopt heat-pump rectifying process, can cut down the consumption of energy greatly, and a year economic benefit improves greatly.

Description of drawings

Fig. 1: high purity trichlorosilane by using heat pump distillation production method schema of the present invention.

Embodiment

Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail.

As shown in Figure 1: comprise lightness-removing column (1), lightness-removing column reboiler (4), condenser of light component removal column (3), lightness-removing column surge tank (7), lightness-removing column compressor (9), lightness-removing column dropping valve (18), heat pump (14), weight-removing column (2), weight-removing column condenser (5), weight-removing column surge tank (8), weight-removing column compressor (10), weight-removing column reboiler (6), weight-removing column dropping valve (24); It is characterized in that: opening for feed is established at lightness-removing column (1) middle part, pipeline of lightness-removing column bottoms stream and the bottom of returning lightness-removing column (1) after lightness-removing column reboiler (4) is connected, another pipeline links to each other with the middle part of weight-removing column through pump (14), lightness-removing column (1) overhead stream links to each other with lightness-removing column surge tank (7) behind condenser of light component removal column (3), and lightness-removing column surge tank (7) outlet at bottom is provided with feed back and material extraction; Condenser of light component removal column (3) one ends link to each other with lightness-removing column reboiler (4) through lightness-removing column compressor (9) by pipeline, lightness-removing column reboiler (4) the other end links to each other with condenser of light component removal column (3) one ends through lightness-removing column dropping valve (18), forms the lightness-removing column heat pump circulating system; Weight-removing column (2) tower base stream and the bottom of returning weight-removing column (2) after weight-removing column reboiler (6) is connected, weight-removing column (2) overhead stream links to each other with weight-removing column surge tank (8) behind weight-removing column condenser (5), and weight-removing column surge tank (8) outlet at bottom is provided with feed back and material extraction; Weight-removing column condenser (5) one ends link to each other with weight-removing column reboiler (6) through weight-removing column compressor (10) by pipeline, weight-removing column reboiler (6) the other end links to each other with weight-removing column condenser (5) one ends through weight-removing column dropping valve (24), forms the weight-removing column heat pump circulating system.

Trichlorosilane stock liquid (11) enters the middle part of lightness-removing column (1), returns lightness-removing column (1) through trichlorosilane solution (a 12) part at the bottom of the tower after taking off gently through lightness-removing column reboiler (4); Another part is squeezed into weight-removing column (2) by pump (14) and is taken off heavily; Lightness-removing column overhead gas phase materials (13) main component is dichloro-dihydro silicon and micro-light impurity, after condenser of light component removal column (3) cooling, enter lightness-removing column surge tank (7), return lightness-removing column (1), a part of extraction from the effusive material part of lightness-removing column surge tank (7); Weight-removing column cat head gas-phase product (15) enters weight-removing column surge tank (8) behind weight-removing column condenser (5), be high-purity trichlorosilane from weight-removing column surge tank (8) material that comes out, and wherein a part is returned weight-removing column (2), and a part is as the product extraction.

The heat pump cycle feature of lightness-removing column (1) is: the heat-eliminating medium (20) in the condenser of light component removal column (3) is lightness-removing column gas (21) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of lightness-removing column gas (21) and the temperature, enter lightness-removing column reboiler (4) as tower still thermal source still liquid, and itself condense into lightness-removing column liquid (17), lightness-removing column liquid (17) returns condenser of light component removal column (3) behind expenditure and pressure, finish a circulation; The heat pump cycle feature of weight-removing column (2) is: the heat-eliminating medium (22) in the weight-removing column condenser (5) is weight-removing column gas (23) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of weight-removing column gas (23) and the temperature, enter weight-removing column reboiler (6) as tower still thermal source still liquid, and itself condense into weight-removing column liquid (19), weight-removing column liquid (19) returns weight-removing column condenser (5) behind expenditure and pressure, finish a circulation.

The lightness-removing column reflux ratio is 20-50, and the weight-removing column reflux ratio is 3-10.Lightness-removing column pressure is 300KPa, and tower top temperature is controlled at 60~70 ℃, and the temperature difference is in 10 degree at the bottom of the cat head tower.Weight-removing column pressure is 600KPa, and tower top temperature is controlled at 80~90 ℃, and the temperature difference is controlled in 10 degree at the bottom of the cat head tower.

Embodiment 1

The purification of processing trichlorosilane in 2000 tons of/year production of polysilicon is an example.Production equipment comprises lightness-removing column, weight-removing column and thermal-pump unit, and Liang Tashang is respectively arranged with condenser and reboiler, and condenser one end joins by compressed machine of pipeline and reboiler in the thermal-pump unit, and the reboiler the other end joins through reducing valve and condenser one end.Wherein lightness-removing column pressure is 300KPa, and tower top temperature is 60 ℃, and reflux ratio is 20; Weight-removing column pressure is 600KPa, and tower top temperature is 80 ℃, and reflux ratio is 3.

Press 8000h/ and calculate working time in year, and the steam price is by 150 yuan of/ton calculating, and electricity price is by 0.5 yuan/Kwh, and water price is pressed 2.0 yuan of/ton calculating:

After adopting heat pump technology, compare with common process:

Embodiment 2

The purification of processing trichlorosilane in 1000 tons of/year production of polysilicon is an example.Production equipment comprises lightness-removing column, weight-removing column and thermal-pump unit, and Liang Tashang is respectively arranged with condenser and reboiler, and condenser one end joins by compressed machine of pipeline and reboiler in the thermal-pump unit, and the reboiler the other end joins through reducing valve and condenser one end.Wherein lightness-removing column pressure is 300KPa, and tower top temperature is 70 ℃, and reflux ratio is 50; Weight-removing column pressure is 600KPa, and tower top temperature is 90 ℃, and reflux ratio is 10.

Press 8000h/ and calculate working time in year, and the steam price is by 150 yuan of/ton calculating, and electricity price is by 0.5 yuan/Kwh, and water price is pressed 2.0 yuan of/ton calculating:

Heat pump technology is compared with common process:

Claims (7)

1. a high purity trichlorosilane by using heat pump distillation production equipment comprises lightness-removing column (1), lightness-removing column reboiler (4), condenser of light component removal column (3), lightness-removing column surge tank (7), lightness-removing column compressor (9), lightness-removing column dropping valve (18), heat pump (14), weight-removing column (2), weight-removing column condenser (5), weight-removing column surge tank (8), weight-removing column compressor (10), weight-removing column reboiler (6), weight-removing column dropping valve (24); It is characterized in that: opening for feed is established at lightness-removing column (1) middle part, pipeline of lightness-removing column bottoms stream and the bottom of returning lightness-removing column (1) after lightness-removing column reboiler (4) is connected, another pipeline links to each other with the middle part of weight-removing column through pump (14), lightness-removing column (1) overhead stream links to each other with lightness-removing column surge tank (7) behind condenser of light component removal column (3), and lightness-removing column surge tank (7) outlet at bottom is provided with feed back and material extraction; Condenser of light component removal column (3) one ends link to each other with lightness-removing column reboiler (4) through lightness-removing column compressor (9) by pipeline, lightness-removing column reboiler (4) the other end links to each other with condenser of light component removal column (3) one ends through lightness-removing column dropping valve (18), forms the lightness-removing column heat pump circulating system; Weight-removing column (2) tower base stream and the bottom of returning weight-removing column (2) after weight-removing column reboiler (6) is connected, weight-removing column (2) overhead stream links to each other with weight-removing column surge tank (8) behind weight-removing column condenser (5), and weight-removing column surge tank (8) outlet at bottom is provided with feed back and material extraction; Weight-removing column condenser (5) one ends link to each other with weight-removing column reboiler (6) through weight-removing column compressor (10) by pipeline, weight-removing column reboiler (6) the other end links to each other with weight-removing column condenser (5) one ends through weight-removing column dropping valve (24), forms the weight-removing column heat pump circulating system.
2. device as claimed in claim 1 is characterized in that heat pump adopts the enclosed heat pump.
3. high purity trichlorosilane by using heat pump distillation production method: trichlorosilane stock liquid (11) enters the middle part of lightness-removing column (1), returns lightness-removing column (1) through trichlorosilane solution (a 12) part at the bottom of taking off the tower after light through lightness-removing column reboiler (4); Another part is squeezed into weight-removing column (2) by pump (14) and is taken off heavily; Lightness-removing column overhead gas phase materials (13) main component is dichloro-dihydro silicon and micro-light impurity, after condenser of light component removal column (3) cooling, enter lightness-removing column surge tank (7), return lightness-removing column (1), a part of extraction from the effusive material part of lightness-removing column surge tank (7); Weight-removing column cat head gas-phase product (15) enters weight-removing column surge tank (8) behind weight-removing column condenser (5), be high-purity trichlorosilane from weight-removing column surge tank (8) material that comes out, and wherein a part is returned weight-removing column (2), and a part is as the product extraction.
4. production method as claimed in claim 3, the heat pump cycle feature of lightness-removing column (1) is: the heat-eliminating medium (20) in the condenser of light component removal column (3) is lightness-removing column gas (21) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of lightness-removing column gas (21) and the temperature, enter lightness-removing column reboiler (4) as tower still thermal source still liquid, and itself condense into lightness-removing column liquid (17), lightness-removing column liquid (17) returns condenser of light component removal column (3) behind expenditure and pressure, finish a circulation; The heat pump cycle feature of weight-removing column (2) is: the heat-eliminating medium (22) in the weight-removing column condenser (5) is weight-removing column gas (23) with cat head end material heat exchange post-absorption heat of vaporization, after compressed pressurize of weight-removing column gas (23) and the temperature, enter weight-removing column reboiler (6) as tower still thermal source still liquid, and itself condense into weight-removing column liquid (19), weight-removing column liquid (19) returns weight-removing column condenser (5) behind expenditure and pressure, finish a circulation.
5. the high purity trichlorosilane by using heat pump distillation device working method of claim 3, the lightness-removing column reflux ratio is 20-50, the weight-removing column reflux ratio is 3-10.
6. method as claimed in claim 3 is characterized in that lightness-removing column pressure is 300KPa, and tower top temperature is controlled at 60~70 ℃, and the temperature difference is in 10 degree at the bottom of the cat head tower.
7. method as claimed in claim 3 is characterized in that weight-removing column pressure is 600KPa, and tower top temperature is controlled at 80~90 ℃, and the temperature difference is controlled in 10 degree at the bottom of the cat head tower.
CN2009102286356A 2009-11-20 2009-11-20 Production device and method of high purity trichlorosilane by using heat pump distillation CN101704524B (en)

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CN101955187A (en) * 2010-10-21 2011-01-26 天津大学 Method and apparatus for preparing trichlorosilane through reaction rectification by using proportionate reaction
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CN102451572A (en) * 2010-11-03 2012-05-16 中国石油化工股份有限公司 Method for separating acetic acid from water by rectification of acetic acid dehydrating tower
CN102452927A (en) * 2010-11-03 2012-05-16 中国石油化工股份有限公司 Method for separating acetic acid from water
CN102452925A (en) * 2010-11-03 2012-05-16 中国石油化工股份有限公司 Method for separating acetic acid from water
CN102452924B (en) * 2010-11-03 2014-04-30 中国石油化工股份有限公司 Method for separating acetic acid from water by acetic acid dehydration tower
CN102452925B (en) * 2010-11-03 2014-04-02 中国石油化工股份有限公司 Method for separating acetic acid from water
CN102452926A (en) * 2010-11-03 2012-05-16 中国石油化工股份有限公司 Method for separating acetic acid and water
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CN102134080B (en) * 2011-04-12 2012-07-04 天津大学 Heat-pump energy-saving separating device for extracting trichlorosilane by adopting static mixing booster and method
CN102153092A (en) * 2011-04-27 2011-08-17 天津大学 Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane
CN102153092B (en) * 2011-04-27 2012-12-26 天津大学 Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane
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