CN203922737U - The desorption apparatus of non-condensable gas in a kind of chlorosilane - Google Patents
The desorption apparatus of non-condensable gas in a kind of chlorosilane Download PDFInfo
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- CN203922737U CN203922737U CN201420324751.4U CN201420324751U CN203922737U CN 203922737 U CN203922737 U CN 203922737U CN 201420324751 U CN201420324751 U CN 201420324751U CN 203922737 U CN203922737 U CN 203922737U
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Abstract
The utility model relates to a kind of desorption apparatus of chlorosilane non-condensable gas, comprise four condensers, compressor, two interchanger, desorption tower, two washing towers, First Heat Exchanger is connected with the first washing tower, the first washing tower is connected with the first condenser, the first condenser is connected with compressor, compressor is connected with the second washing tower, the second washing tower is connected with First Heat Exchanger, the second washing tower is connected with the second condenser, the second condenser is connected with the second interchanger, the second interchanger is connected with the 3rd condenser, the 3rd condenser is connected with the 4th condenser, described the first washing tower, the second washing tower, the second interchanger, the 3rd condenser is all connected with desorption tower with the 4th condenser, desorption tower is connected with reboiler.This desorption apparatus of the utility model takes full advantage of the waste heat in gas mixture, has greatly reduced the energy consumption of whole technique, can also ensure simultaneously silane after desorb containing the amount of non-condensable gas below 5ppm.
Description
Technical field
The utility model relates to the purifying plant of chlorosilane raw material in a kind of production of polysilicon technique, relates in particular to the desorption apparatus of non-condensable gas in a kind of chlorosilane.
Background technology
Chlorosilane (including but not limited to the general designation of silicon tetrachloride, trichlorosilane, dichlorosilane) mostly is gas-phase reaction in actual production, conventionally and hydrogen, hydrogenchloride etc. leave reactor with gas mixture form.In chlorosilane, be dissolved with the non-condensable gas of more amount, the chlorosilane that contains non-condensable gas is unfavorable for the production of polysilicon, therefore, and at the industrial non-condensable gas (including but not limited to hydrogen, hydrogenchloride, nitrogen) that all can remove as much as possible in chlorosilane.To these gas phase chlorosilanes carry out multi-stage condensing, pressurization, the mode of multi-stage condensing completes substantially separating of chlorosilane and non-condensable gas (including but not limited to hydrogen, hydrogenchloride, nitrogen) again.Polysilicon enterprise adopts-35 DEG C of cold à-65 of freonll-11 cold modes of DEG C freonll-11 of recirculated water cooling à low temperature water-cooled à pressurization that chlorosilane is separated with noncondensable gas conventionally, and in different process, the control of temperature and condensation progression is formulated according to practical situation.When the mode of employing condensation is removed the non-condensable gas (including but not limited to hydrogen, hydrogenchloride, nitrogen) in chlorosilane, non-condensable gas (including but not limited to hydrogen, hydrogenchloride, nitrogen) chlorosilane can dissolve again part non-condensable gas, and wherein silicon tetrachloride component is fairly obvious to the dissolving of non-condensable gas.For example, 15000kg chlorosilane mixed solution (silicon tetrachloride massfraction 0.78) dissolves the about 30Nm of hydrogen at 2.5MPaG-30 DEG C
3.The non-condensable gas of these dissolvings can produce larger impact to polysilicon follow-up producing process, therefore, industrially all can take measures to remove the non-condensable gas in chlorosilane, and the existing non-condensable gas of removing in chlorosilane mainly contains following several method:
1, rectifying tower tail cold process, this method is in the time that chlorosilane mixed solution is separated, and adds cryogenic heat exchanger (below 20 DEG C) after overhead condenser, non-condensable gas discharges with gas phase from cryogenic heat exchanger.The method advantage is that increase equipment is few, and desorption effect is good, and has utilized rectifying tower to complete the thermal load of rectification and purification, does not increase steam consumption, and shortcoming is that cryogenic heat exchanger (conventionally providing cold by freon set) load is large, power consumption is high.
2, flash distillation storage tank directly adds cryogenic heat exchanger method, this method be utilize large-size horizontal storage tank after decompression (0.05-1MPaG) to exporting and add chlorosilane in cryogenic heat exchanger gas recovery containing the free flash distillation of non-condensable gas chlorosilane and at flashed vapour, advantage is to utilize original storage tank additionally to increase interchanger, invest little and substantially without operation.Shortcoming is that desorption effect is poor, and a large amount of non-condensable gases is still present in chlorosilane mixed solution.
3, flash distillation storage tank directly adds cryogenic heat exchanger method+rectifying tower tail cold process, first adopt flash distillation storage tank directly to add cryogenic heat exchanger method remove portion non-condensable gas, then adopt rectifying tower tail cold process to continue to remove remaining non-condensable gas, this method has advantages of method 1 and 2, degassing effect is better, and shortcoming is that cryogenic heat exchanger (conventionally providing cold by freon set) load is large, power consumption is high.
4, desorption tower method, desorption tower method is the device for chlorosilane, hydrogen and the HCl separation of polysilicon reduction tail gas, its structure and rectifying tower tail cold process are basic identical, difference is that desorption tower is without different chlorosilane components is separated, can significantly reduce top gaseous phase temperature, reduce tower top refrigerant consumption.Therefore desorption tower method has obtained general application.
As shown in Figure 1, the concrete technology step of desorption tower method is: the gas mixture that reaction unit is brought carries out, after water-setting (completing with water cooler), compression (completing with compressor), water-setting (completing with water cooler), heat exchange (completing with interchanger), a condensation (completing with condenser) and time condensation (completing with condenser), separating out non-condensable gas successively.The material that in water-setting, secondary water-setting, heat exchange, a condensation and a time condensation, condensation is got off is sent in desorption tower, the material of desorption tower tower top is carried out to three water-settings (completing with water cooler) and three condensations (completing with condenser) separates out after stripping gas is discharged and is sent in desorption tower, material below desorption tower is sent in reboiler to be processed, and obtains chlorosilane.
There is following defect in this desorption method: the temperature of reaction unit gas mixture out exceedes 100 DEG C, mixing tank is directly carried out water-setting by the method, waste the heat in mixing tank, also increased the burden of water cooler simultaneously, the waste heat in gas mixture is not made full use of, increased the energy consumption of whole technique.And directly mixing tank being carried out to condensation, undercooling can increase the meltage of non-condensable gas in silane, and non-condensable gas is dissolved in silane, is unfavorable for separating out of non-condensable gas; Mixed gas after compression directly carries out condensation, makes undercooling, and non-condensable gas is further dissolved in silane, is also unfavorable for separating out of non-condensable gas; Condensing equipment has been set up at the desorption tower top of the method, makes desorption tower complex structure, and cold consumption is large, and power consumption is large.
utility model content
In order to overcome the defect of above-mentioned chlorosilane non-condensable gas desorption method, the utility model provides the desorption apparatus of non-condensable gas in a kind of chlorosilane, this desorption apparatus takes full advantage of the waste heat in gas mixture, greatly reduced the energy consumption of whole technique, can also ensure simultaneously silane after desorb containing the amount of non-condensable gas below 5ppm.
The desorption apparatus of non-condensable gas in a kind of chlorosilane, comprise four condensers, compressor, two interchanger and desorption tower, it is characterized in that: also comprise two washing towers, four condensers are respectively the first condenser, the second condenser, the 3rd condenser and the 4th condenser, two interchanger are respectively First Heat Exchanger and the second interchanger, two washing towers are respectively the first washing tower and the second washing tower, First Heat Exchanger is connected with the first washing tower, the first washing tower is connected with the first condenser, the first condenser is connected with compressor, compressor is connected with the second washing tower, the second washing tower is connected with First Heat Exchanger, the second washing tower is connected with the second condenser, the second condenser is connected with the second interchanger, the second interchanger is connected with the 3rd condenser, the 3rd condenser is connected with the 4th condenser, described the first washing tower, the second washing tower, the second interchanger, the 3rd condenser is all connected with desorption tower with the 4th condenser, desorption tower is connected with reboiler.
The first condenser is the first water cooling plant, this first water cooling plant comprises the first recirculated water cooler and the first water at low temperature water cooler, the discharge port of the first recirculated water cooler is connected with the opening for feed of the first water at low temperature cooler, the opening for feed of the first recirculated water cooler is connected with the first washing tower, and the discharge port of the first low temperature cold hydrophone is connected with compressor.
The second condenser is the second water cooling plant, this second water cooling plant comprises the second recirculated water cooler and the second water at low temperature water cooler, the discharge port of the second recirculated water cooler is connected with the opening for feed of the second water at low temperature cooler, the opening for feed of the second recirculated water cooler is connected with the second washing tower, and the discharge port of the second low temperature cold hydrophone is connected with the second interchanger.
The utlity model has following advantage:
1, the utility model comprises four condensers, compressor, two interchanger and desorption tower, it is characterized in that: also comprise two washing towers, four condensers are respectively the first condenser, the second condenser, the 3rd condenser and the 4th condenser, two interchanger are respectively First Heat Exchanger and the second interchanger, two washing towers are respectively the first washing tower and the second washing tower, First Heat Exchanger is connected with the first washing tower, the first washing tower is connected with the first condenser, the first condenser is connected with compressor, compressor is connected with the second washing tower, the second washing tower is connected with First Heat Exchanger, the second washing tower is connected with the second condenser, the second condenser is connected with the second interchanger, the second interchanger is connected with the 3rd condenser, the 3rd condenser is connected with the 4th condenser, described the first washing tower, the second washing tower, the second interchanger, the 3rd condenser is all connected with desorption tower with the 4th condenser, desorption tower is connected with reboiler.The utility model has been set up two washing towers and an interchanger at the desorption apparatus of existing chlorosilane non-condensable gas, the Produced Liquid in two washing towers and gas mixture are carried out heat exchange by effect by interchanger, take full advantage of the waste heat in gas mixture, while making gas mixture enter into the first condenser again, temperature has dropped between 60-80 DEG C from exceeding 100 DEG C, the benefit of processing is like this: take full advantage of the waste heat in gas mixture, Produced Liquid in two washing towers is carried out to heat exchange, save the energy, reduced hot loss of energy; After process heat exchange, the temperature of gas mixture is between 60-80 DEG C, with respect to exceeding 100 DEG C, liquidus temperature can be excessively not cold, so just can not cause non-condensable gas to be dissolved in chlorosilane yet, make the non-condensable gas desorb in chlorosilane thorough, the amount containing non-condensable gas in guarantee chlorosilane is below 5ppm.Due to the washing tower that the utility model arranges, make desorption tower tower top no longer set up interchanger and condenser just can obtain the chlorosilane that purity is high, simplify desorption tower, thereby also reduced energy consumption.
2, the utility model the first condenser and the second condenser are water cooling plant, and this water cooling plant comprises recirculated water cooler and water at low temperature water cooler, and recirculated water cooler and water at low temperature cooler link together.The condenser condenses of this spline structure is effective, and liquid phase can be excessively not cold, reduces the meltage of non-condensable gas in chlorosilane, and the amount containing non-condensable gas in guarantee chlorosilane is below 5ppm.
Brief description of the drawings
Fig. 1 is the one-piece construction schematic diagram of prior art;
Fig. 2 is one-piece construction schematic diagram of the present utility model.
Mark 1. gas mixtures, 2. chlorosilane liquid, 3. non-condensable gas in figure, 4. stripping gas, 5. the first condenser, 6. compressor 7. second condensers, 8. the second interchanger, 9. the 3rd condenser, 10. the 4th condenser, 11. desorption towers, 12. reboilers, 13. First Heat Exchangers, 14. first washing towers, 15. second washing towers.
Embodiment
The utility model comprises four condensers, compressor 6, two interchanger, desorption tower 11 and two washing towers, four condensers are respectively the first condenser 5, the second condenser 7, the 3rd condensation 9 and the 4th condenser 10, two interchanger are respectively First Heat Exchanger 13 and the second interchanger 8, two washing towers are respectively the first washing tower 14 and the second washing tower 15, First Heat Exchanger 13 is connected with the first washing tower 14, the first washing tower 14 is connected with the first condenser 5, the first condenser 5 is connected with compressor 6, compressor 6 is connected with the second washing tower 15, the second washing tower 15 is connected with First Heat Exchanger 8, the second washing tower 15 is connected with the second condenser 7, the second condenser 7 is connected with the second interchanger 8, the second interchanger 8 is connected with the 3rd condenser 9, the 3rd condenser 9 is connected with the 4th condenser 10, described the first washing tower 14, the second washing tower 15, the second interchanger 8, the 3rd condenser 9 is all connected with desorption tower 11 with the 4th condenser 10, desorption tower 11 is connected with reboiler 12.
The first condenser is the first water cooling plant, this first water cooling plant comprises the first recirculated water cooler and the first water at low temperature water cooler, the discharge port of the first recirculated water cooler is connected with the opening for feed of the first water at low temperature cooler, the opening for feed of the first recirculated water cooler is connected with the first washing tower, and the discharge port of the first low temperature cold hydrophone is connected with compressor.
The second condenser is the second water cooling plant, this second water cooling plant comprises the second recirculated water cooler and the second water at low temperature water cooler, the discharge port of the second recirculated water cooler is connected with the opening for feed of the second water at low temperature cooler, the opening for feed of the second recirculated water cooler is connected with the second washing tower, and the discharge port of the second low temperature cold hydrophone is connected with the second interchanger.
The gas mixture 1 and the first washing tower 14, the second washing tower 15 Produced Liquids that exceed 100 DEG C carry out heat exchange at First Heat Exchanger 13.After exchange, mixture temperature is between 60-80 DEG C, then after entering the first washing tower 14 washings, obtain mixed chlorosilane liquid in First Heat Exchanger 13 places condensation, this part mixed chlorosilane all returns to the first washing tower 14 tops, enters into desorption tower 11 by pipeline.
After entering the second washing tower 15 washings, obtain mixed chlorosilane liquid in the second condenser 7 condensations and utilize compressor 6 to be forced into (concrete pressure selection allows content to determine according to the maximum of chlorosilane in required non-condensable gas) 0.8-1.5MPaG from the isolated gas phase of First Heat Exchanger 13, this part mixed chlorosilane liquid all returns to the second washing tower 15 tops, enters into desorption tower 11 by pipeline.
Carry out heat exchange from the isolated gas phase of the second condenser 7 at the second interchanger 8, the mixed chlorosilane liquid that condensation obtains all enters into desorption tower 11 by pipeline.And gas phase in the second interchanger 8 continuously after the 3rd condenser 9 and the 4th condenser 10 temperature be down to-65 DEG C of left and right and obtain chlorosilane content and be less than 0.05%(molar fraction) non-condensable gas; And the mixed chlorosilane liquid that the 3rd condenser 9 and the 4th condenser 10 condensations obtain all enters into desorption tower 11 by pipeline.
All mixed chlorosilane liquid that enters into desorption tower 11, by the effect of desorption tower 11, gas phase is discharged and is obtained stripping gas 4, and liquid phase enters into reboiler 12 and processes, and obtains chlorosilane solution 2.
The utility model takes full advantage of the calorific value of original gaseous phase materials, avoid replacing cold and hot power loss, evade the situation that undercooling that former heat exchanger type temperature control condensation meeting causes dissolves more non-condensable gas simultaneously, ensured that the chlorosilane mixed solution non-condensable gas content after desorb is in 5ppm.The utility model is different from the general the most special place of technique and is the utilization of using waste heat from tail gas and setting up of washing tower.Desorption tower is according to the difference of temperature, multiple feed, thus can cancel desorption tower tower top interchanger, simplify desorption tower, also reduced the consumption of the energy simultaneously.
The washing tower that front end of the present utility model is set up has fully been saved the front end cold of former condenser system, has reached the object that improves liquid-phase chlorosilane temperature by such mode of washing.The condensing equipment of tower top has been removed in the condensation of differing temps and the cold consumption of entering respectively desorption tower and also reduced desorb tower top simultaneously.
Claims (3)
1. the desorption apparatus of non-condensable gas in a chlorosilane, comprise four condensers, compressor, two interchanger and desorption tower, it is characterized in that: also comprise two washing towers, four condensers are respectively the first condenser, the second condenser, the 3rd condenser and the 4th condenser, two interchanger are respectively First Heat Exchanger and the second interchanger, two washing towers are respectively the first washing tower and the second washing tower, First Heat Exchanger is connected with the first washing tower, the first washing tower is connected with the first condenser, the first condenser is connected with compressor, compressor is connected with the second washing tower, the second washing tower is connected with First Heat Exchanger, the second washing tower is connected with the second condenser, the second condenser is connected with the second interchanger, the second interchanger is connected with the 3rd condenser, the 3rd condenser is connected with the 4th condenser, described the first washing tower, the second washing tower, the second interchanger, the 3rd condenser is all connected with desorption tower with the 4th condenser, desorption tower is connected with reboiler.
2. the desorption apparatus of non-condensable gas in a kind of chlorosilane according to claim 1, it is characterized in that: the first condenser is the first water cooling plant, this first water cooling plant comprises the first recirculated water cooler and the first water at low temperature water cooler, the discharge port of the first recirculated water cooler is connected with the opening for feed of the first water at low temperature cooler, the opening for feed of the first recirculated water cooler is connected with the first washing tower, and the discharge port of the first low temperature cold hydrophone is connected with compressor.
3. the desorption apparatus of non-condensable gas in a kind of chlorosilane according to claim 1 and 2, it is characterized in that: the second condenser is the second water cooling plant, this second water cooling plant comprises the second recirculated water cooler and the second water at low temperature water cooler, the discharge port of the second recirculated water cooler is connected with the opening for feed of the second water at low temperature cooler, the opening for feed of the second recirculated water cooler is connected with the second washing tower, and the discharge port of the second low temperature cold hydrophone is connected with the second interchanger.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420324751.4U CN203922737U (en) | 2014-06-18 | 2014-06-18 | The desorption apparatus of non-condensable gas in a kind of chlorosilane |
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| CN201420324751.4U CN203922737U (en) | 2014-06-18 | 2014-06-18 | The desorption apparatus of non-condensable gas in a kind of chlorosilane |
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| CN203922737U true CN203922737U (en) | 2014-11-05 |
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| CN201420324751.4U Active CN203922737U (en) | 2014-06-18 | 2014-06-18 | The desorption apparatus of non-condensable gas in a kind of chlorosilane |
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