CN203754435U - System of purifying chlorosilane by use of differential pressure thermal coupling of uncorrelated towers - Google Patents
System of purifying chlorosilane by use of differential pressure thermal coupling of uncorrelated towers Download PDFInfo
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- CN203754435U CN203754435U CN201420151795.1U CN201420151795U CN203754435U CN 203754435 U CN203754435 U CN 203754435U CN 201420151795 U CN201420151795 U CN 201420151795U CN 203754435 U CN203754435 U CN 203754435U
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- 230000008878 coupling Effects 0.000 title claims abstract description 49
- 238000010168 coupling process Methods 0.000 title claims abstract description 49
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 49
- 239000005046 Chlorosilane Substances 0.000 title claims abstract description 17
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 238000004821 distillation Methods 0.000 claims description 60
- 238000010992 reflux Methods 0.000 claims description 36
- 238000000746 purification Methods 0.000 claims description 32
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000460 chlorine Substances 0.000 claims description 21
- 229910052801 chlorine Inorganic materials 0.000 claims description 21
- 229910000077 silane Inorganic materials 0.000 claims description 21
- 230000008676 import Effects 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 16
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 19
- 238000005265 energy consumption Methods 0.000 abstract description 18
- 238000009833 condensation Methods 0.000 description 24
- 230000005494 condensation Effects 0.000 description 24
- 239000000463 material Substances 0.000 description 21
- 238000000605 extraction Methods 0.000 description 18
- 230000009467 reduction Effects 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 15
- 229920005591 polysilicon Polymers 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 238000011084 recovery Methods 0.000 description 11
- 230000008016 vaporization Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 5
- 239000000470 constituent Substances 0.000 description 5
- 238000005984 hydrogenation reaction Methods 0.000 description 5
- 239000005049 silicon tetrachloride Substances 0.000 description 5
- 238000009834 vaporization Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 4
- 239000005052 trichlorosilane Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000006870 function Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 206010019332 Heat exhaustion Diseases 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model discloses a system of purifying chlorosilane by use of differential pressure thermal coupling of uncorrelated towers. The system comprises first and second rectifying towers each of which is provided with a feed inlet, a gas outlet, a liquid outlet, a liquid inlet and a gas inlet, first and second reboilers each of which is provided with a liquid inlet, a gas outlet, a steam inlet and a condensate outlet, first and second return pumps each of which is provided with an inlet and a pump outlet, first and second return tanks each of which is provided with a tank inlet and a tank outlet, and a condenser which is provided with a gas inlet, a liquid outlet, a cold source inlet and a cold source outlet. Compared with conventional serial or parallel differential pressure thermal coupling rectifying towers, the system of purifying chlorosilane disclosed by the utility model can be used for realizing differential pressure thermal coupling of the towers among different tower sets, so that the range of application of differential pressure thermal coupling is expanded, thereby solving the problem that the purifying step in a polycrystalline silicon system is high in energy consumption.
Description
Technical field
The utility model relates to field polysilicon, and particularly, the utility model relates to the system of onrelevant tower differential pressure heat coupling chlorine purification silane.
Background technology
Polysilicon is a kind of ultra-pure material, for unicircuit, electron device and solar cell, is the foundation stone of information and New Energy Industry, is that country encourages the strategic material of first developing, and is also the Product and industry of state key encourage growth.
2012, be subject to two anti-impacts of global economic crisis and European Union, how the continued downturn of polysilicon market, reduce production of polysilicon cost, how to enhance the core competitiveness of enterprises, and becomes the top priority of the long-term sustainable development of each polysilicon enterprise.
The main production method of current domestic polysilicon is improved Siemens, mainly comprises that trichlorosilane is synthetic, rectification and purification, reduction, reduction tail gas dry process reclaim and five operations of hydrogenation.Wherein, rectification and purification and each operation are closely related, process each operation material or supply raw materials for each operation, therefore purification system comprises the different tower groups of processing various materials, and refined product purity and foreign matter content are had relatively high expectations, must need relatively high heat exhaustion, the energy consumption of purification process is one of main energy consumption of polysilicon system, and the energy consumption that therefore reduces purification process is one of effective way reducing polysilicon cost.
Though at present some tower group of rectification and purification has adopted differential pressure heat coupling, has reduced energy consumption, all adopts series system, can not ensure each tower differential pressure heat coupling in tower group, and some tower group do not possess differential pressure heat coupling condition, therefore can not farthest reduce energy consumption.
Utility model content
The utility model is intended to solve at least to a certain extent one of technical problem in correlation technique.For this reason, an object of the present utility model is to propose a kind of system of onrelevant tower differential pressure heat coupling chlorine purification silane.
According to an aspect of the present utility model, the utility model proposes a kind of system of onrelevant tower differential pressure heat coupling chlorine purification silane, comprising:
The first rectifying tower and Second distillation column, each rectifying tower in described the first rectifying tower and Second distillation column all has the opening for feed, air outlet, liquid outlet, fluid inlet and the inlet mouth that are positioned on this rectifying tower;
The first reboiler and the second reboiler, each reboiler in described the first reboiler and the second reboiler all has and is positioned at fluid inlet, air outlet, steam inlet and condensate outlet on this reboiler,
The first reflux pump and the second reflux pump, each reflux pump in described the first reflux pump and the second reflux pump all has the import and the pump discharge that are positioned on this reflux pump;
The first return tank and the second return tank, each return tank in described the first return tank and the second return tank all has the tank import and the tank outlet that are positioned on this return tank;
A condenser, a described condenser has inlet mouth, liquid outlet, low-temperature receiver import and low-temperature receiver outlet;
Wherein,
The air outlet of described the first rectifying tower is connected with the inlet mouth of described condenser, the liquid outlet of described condenser is connected with the tank import of described the first return tank, the tank outlet of described the first return tank is connected with the pump inlet of described the first reflux pump, the pump discharge of described the first reflux pump is connected with the fluid inlet of described the first rectifying tower, to a part of chlorosilane condensate liquid is back to described the first rectifying tower;
The fluid inlet of described the first reboiler and the second reboiler is connected with the liquid outlet of described the first rectifying tower and Second distillation column, to a part for liquid at the bottom of chlorosilane tower is heated and boiled; The air outlet of described the first reboiler and the second reboiler is connected with the inlet mouth of described the first rectifying tower and Second distillation column;
The air outlet of described Second distillation column is connected with the steam inlet of described the first reboiler, the condensate outlet of described the first reboiler is connected with the tank import of described the second return tank, the tank outlet of described the second return tank is connected with the pump inlet of described the second reflux pump, the pump discharge of described the second reflux pump is connected with the fluid inlet of described Second distillation column, to a part for chlorosilane condensate liquid is back to described Second distillation column;
Wherein,
The low-temperature receiver import of described condenser is connected with low-temperature receiver;
The steam inlet of described the second reboiler is connected with thermal source.
The system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model above-described embodiment, extraction at the bottom of the each own charging of the first and second rectifying tower, overhead extraction, tower, and between material without any relation, and then the tower differential pressure heat of having realized between different tower groups is coupled, expand the use range of conventional series connection differential pressure heat coupled, in producing high-purity polycrystalline silicon, the energy consumption of rectification and purification is dropped to minimum.
In embodiment more of the present utility model, the opening for feed of described the first rectifying tower and Second distillation column is connected from different chlorosilane feedwaies respectively.
Brief description of the drawings
Fig. 1 is according to the structural representation of the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of an embodiment of the utility model.
Fig. 2 is according to the structural representation of the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of another embodiment of the utility model.
Fig. 3 is according to the structural representation of the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of another embodiment of the utility model.
Embodiment
Describe embodiment of the present utility model below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Be exemplary below by the embodiment being described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
Describe the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model embodiment in detail below with reference to Fig. 1.
Comprise according to the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model embodiment:
The first rectifying tower T01, Second distillation column T02, the first reboiler E02, the second reboiler E03, the first reflux pump P01, the second reflux pump P02, the first return tank V01, the second return tank V02 and a condenser E01;
Wherein, each rectifying tower in the first rectifying tower T01 and Second distillation column T02 all has the opening for feed T11 and opening for feed T21, air outlet T12 and air outlet T22, liquid outlet T13 and liquid outlet T23, fluid inlet T14 and the fluid inlet T24 that are positioned on this rectifying tower, inlet mouth T15 and inlet mouth T25;
Each in the first reboiler E02 and the second reboiler E03 all has the fluid inlet E21 and E31, air outlet E22 and E32, steam inlet E23 and E33 and condensate outlet E24 and the E34 that are positioned on this reboiler,
Each reflux pump in the first reflux pump P01 and the second reflux pump P02 all has the import P11 and P21 and pump discharge P12 and the P22 that are positioned on this reflux pump;
Each return tank in the first return tank V01 and the second return tank V02 all has the tank import V11 and V21 and tank outlet V12 and the V22 that are positioned on this return tank;
Condenser E01 has inlet mouth E11, liquid outlet E12, low-temperature receiver import and low-temperature receiver outlet (not shown);
According to specific embodiment of the utility model, above-mentioned composition can connect according to following manner:
The air outlet T12 of the first rectifying tower is connected with the inlet mouth E11 of condenser, the liquid outlet E12 of condenser is connected with the tank import V11 of the first return tank, the tank outlet V12 of the first return tank is connected with the pump inlet P11 of the first reflux pump, the pump discharge P12 of the first reflux pump is connected with the fluid inlet T14 of the first rectifying tower, to a part of chlorosilane condensate liquid is back to the first rectifying tower T01, another chlorosilane condensate liquid can extraction;
Fluid inlet E21, the E31 of the first reboiler and the second reboiler is connected with liquid outlet T13, the T23 of the first rectifying tower and Second distillation column respectively successively, to a part for liquid at the bottom of chlorosilane tower is heated and boiled; Air outlet T22, the T32 of the first reboiler and the second reboiler is connected with inlet mouth T15, the T25 of the first rectifying tower and Second distillation column respectively successively;
The air outlet T22 of Second distillation column is connected with the steam inlet E23 of the first reboiler, the condensate outlet E24 of the first reboiler is connected with the tank import V21 of the second return tank, the tank outlet V22 of the second return tank is connected with the pump inlet P21 of the second reflux pump, the pump discharge P22 of the second reflux pump is connected with the fluid inlet T24 of Second distillation column, to a part for chlorosilane condensate liquid is back to Second distillation column;
Wherein,
The low-temperature receiver import of condenser is connected with low-temperature receiver;
The steam inlet of the second reboiler is connected with thermal source.
According to specific embodiment of the utility model, there is extraction at the bottom of the each own charging of each rectifying tower in the system of onrelevant tower differential pressure heat coupling chlorine purification silane of said structure, overhead extraction, tower, and between material without any relation, realize the tower differential pressure heat coupling between different tower groups, expand the use range of conventional series connection differential pressure heat coupled, especially in producing high-purity polycrystalline silicon, the energy consumption of rectification and purification is dropped to minimum.Compared with simple coupling rectification technique, Energy Intensity Reduction is up to 50%, has solved the problem of purification process high energy consumption in polysilicon system, reduces enterprise's production cost, enhances the core competitiveness of enterprises.
According to specific embodiment of the utility model, the temperature of the low-temperature receiver being connected with the low-temperature receiver import (not shown) of condenser E01 can be 32～42 degrees Celsius.Low-temperature receiver particular type is also not particularly limited, for example, can be the recirculated water of 32～42 degrees Celsius.The temperature of the thermal source being connected with the steam inlet E23 of the second reboiler E03 can be 150 degrees Celsius.The type of thermal source is also not particularly limited, and for example thermal source can adopt and in polysilicon system, reduce the high-temperature water of 150 degrees Celsius obtaining after the using as low-temperature receiver of operation.The low-temperature receiver reducing in polysilicon system in operation, after reduction operation, be elevated to 150 degrees Celsius by 130 degrees Celsius, therefore it directly can be used as the thermal source of above-mentioned the second reboiler, after the second reboiler cooling, temperature is about 130 degree, its recycling can be returned to again to reduction operation as low-temperature receiver.Thus, whole polysilicon system is accomplished to heat rationally utilizes, significantly saved energy consumption.
Therefore, the system of the onrelevant tower differential pressure heat of the utility model above-described embodiment coupling chlorine purification silane only need to provide low-temperature receiver and thermal source for condenser E01 and two devices of the second reboiler E03, and mutually makes full use of by internal system cold and heat.According to the chlorosilane purification system of above-described embodiment of the present utility model, can make full use of heat coupling, the thermal source of the first reboiler mating and required condenser and the low-temperature receiver of Second distillation column with the first rectifying tower are saved, therefore, utilize the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of above-described embodiment can maximumly save 50% energy consumption.
According to specific embodiment of the utility model, the tower top temperature of the first rectifying tower is not less than 55 degrees Celsius, and the tower top temperature of Second distillation column is not higher than 120 degrees Celsius.According to another specific embodiment of the present utility model, the pressure in the first rectifying tower is 0.05～0.7MPa; Pressure in Second distillation column is 0.3～1.2MPa.Can make thus can be coupled well between the first rectifying tower and Second distillation column, farthest reduce the energy consumption in polycrystalline silicon purifying operation.
According to specific embodiment of the utility model, the tower top temperature difference of the tower reactor of the first rectifying tower and Second distillation column is 10～50 degrees Celsius.If the temperature difference within the scope of this, do not put up with can not be coupled or remarkably influenced coupling effect, if Second distillation column tower top and the first tower bottom of rectifying tower temperature difference are lower than 10 degrees Celsius conventionally, will cause two material-heat-exchanging difficulties, cause the first reboiler area larger simultaneously, and then increase investment.If excessive temperature differentials, can cause such as exceeding 50 degree that the tower reactor temperature of Second distillation column is higher even exceedes 120 degrees Celsius, and then can cause the temperature difference of thermal source (150 spend into-130 spend) of Second distillation column still and the second reboiler less, make heat exchange difficulty, cause Second distillation column reboiler area larger.For example, if the first 60 degrees Celsius of rectifying tower tower tops, 65 degrees Celsius of tower reactor possibilities, if 50 degrees Celsius of the temperature difference, second group of rectifying tower tower top is 110 degrees Celsius, 115 degrees Celsius of Second distillation column tower reactors, less with the thermal source temperature out difference of 130 degrees Celsius, the second reboiler area is larger, and then equipment configuration difficulty, and cost is high.
According to specific embodiment of the utility model, the pressure reduction at the bottom of tower top and tower in the first rectifying tower is 0.01～0.1MPa; Pressure reduction at the bottom of tower top and tower in Second distillation column is 0.01～0.1MPa.Can further improve thus the first and second rectifying tower rectification efficiencies, keep above-mentioned pressure reduction can make in the first and second rectifying tower, to there is suitable temperature simultaneously, and then improve the stability of pressure reduction thermal coupling.Avoid pressure reduction larger, such as fixing the first rectifying tower tower top temperature and pressure, the first rectifying tower bottom pressure is higher, corresponding temperature is higher, fix again the first tower bottom of rectifying tower and the Second distillation column tower top temperature difference, the tower top temperature of Second distillation column is higher, higher to this Second distillation column tower top pressure, poor according to tower top tower base pressure, second group of tower bottom of rectifying tower pressure is higher, and corresponding temperature is higher, large the or excess Temperature of second group of rectifying tower reboiler area and then make to heat with common thermal source, cause thermal source energy consumption higher, cost significantly improves.Therefore there is above-mentioned pressure reduction according to the first rectifying tower in the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model embodiment and Second distillation column and can further improve rectification efficiency, reduce energy consumption, maintain the stability of differential pressure heat coupling.
According to specific embodiment of the utility model, the opening for feed of the first rectifying tower and Second distillation column is connected from different chlorosilane feedwaies respectively.That is to say that the first rectifying tower and Second distillation column can be onrelevant tower.For example, the first rectifying tower is the lightness-removing column in topping still group, and Second distillation column is recovery tower.Only need to utilize the heat of the overhead gas condensation of Second distillation column; Suitable with the heat of the first tower bottom of rectifying tower vaporizing liquid; And the tower reactor temperature of Second distillation column tower top temperature and the first rectifying tower meets differential pressure heat coupling needs.
Can be to raise successively or reduction successively according to the pressure of two rectifying tower in the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model embodiment, the function of each rectifying tower can be determined according to the function of this tower place tower group, for example, can take off light or de-heavy.
Press to raise successively taking two rectifying towers below with reference to Fig. 2 and describe the concrete operations flow process of the system of onrelevant tower differential pressure heat coupling chlorine purification silane as example in detail: first, different compositions, two gangs of material S01 of different flow, S10 enters respectively the first rectifying tower T01, the first rectifying tower T02, the overhead vapours S02 of the first rectifying tower is through condenser E01 condensation, phlegma S03 enters return tank V01, phlegma S04 enters reflux pump P01, after pump, a liquid part is returned to the first rectifying tower T01 as phegma S05, the flow of phegma is 1～10 according to backflow charge ratio, after pump, another part liquid S06 can be used as product, light constituent extraction or as the charging of other tower, Produced Liquid S07 at the bottom of tower, according to certain ratio, a part enters condensation reboiler E02, after condensation reboiler heating vaporization, gas S08 returns to the first rectifying tower T01, part Produced Liquid S09 is as product or heavy constituent extraction, the overhead vapours S11 of Second distillation column T02 enters the shell side heating medium entrance of condensation reboiler E02, enter return tank V02 through condensed material S12, phlegma S13 enters reflux pump P02, after pump, a liquid part is returned to Second distillation column tower T02 as phegma S14, the flow of phegma is 1～10 according to backflow charge ratio, after pump, another part liquid S15 is as light constituent or product extraction, Produced Liquid S16 at the bottom of tower, according to certain ratio, a part enters reboiler E03, after reboiler heating vaporization, gas S17 returns to Second distillation column T02, part Produced Liquid S18 can be used as product, heavy constituent extraction or as the charging of other tower.
According to the tower reactor phlegma of the first rectifying tower T01 in the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model embodiment through the first reboiler E02 heating and gasifying, without external heat source, thermal source load reduction 50%; Second distillation column T02 overhead vapours total condensation or excessively cold after the first reboiler E02 condensation, has therefore cancelled the auxiliary condenser of Second distillation column T02, thus the condensation of Second distillation column T02 overhead vapours without additional low-temperature receiver, cold source load reduces by 50%.Therefore make Second distillation column T02 overhead vapours be condensed to the required refrigeration duty of supercooled state suitable with the required thermal load of the first rectifying tower T01 tower reactor vaporizing liquid, can save 50 low-temperature receiver energy consumption and 50% thermal source energy consumption, therefore whole system can reduce by 50% energy consumption, and then can significantly reduce polycrystalline silicon purifying process costs.
Conventionally adopt the conventional differential pressure heat mode that is of coupled connections, for preventing tower fluctuation, cause the heat of Second distillation column overhead gas condensation unsuitable with the heat of the first tower bottom of rectifying tower vaporizing liquid, so Second distillation column need to configure condenser, when occurring that heat is quite time, with condenser by further the material of Second distillation column tower top condensation.For example, taking Second distillation column as example, the flow process of Second distillation column overhead vapours should be Second distillation column → condensation reboiler → auxiliary condenser → return tank → reflux pump, when overhead vapours is in the time that condensation reboiler is condensed into state of saturation, for preventing that in pipeline, non-condensable gas exists, require can not occur in pipeline U-shaped curved, this just requires this serial equipment height progressively to reduce, thereby cause the installation site of condensation reboiler higher, the tower reactor height of the first rectifying tower is higher, and this must increase facility investment and civil engineering risk.
And the system of onrelevant tower differential pressure heat of the present utility model coupling chlorine purification silane can reach the overhead vapours of Second distillation column be condensed into supercooled state after the first reboiler, cancel the auxiliary condenser of Second distillation column T02 tower, and then equipment configuration and pipeline configuration can be subject to the above restrictions, can configure and pipeline configuration difficulty by reduction equipment, expand the use range of differential pressure heat coupled, especially for the tower group of transformation project.
Compared with prior art, have the following advantages according to the system of the onrelevant tower differential pressure heat coupling chlorine purification silane of the utility model above-described embodiment:
(1) onrelevant between two towers of differential pressure heat coupling or three towers, extraction at the bottom of each own charging, overhead extraction, tower, and between material without any relation, realize the tower differential pressure heat coupling between different tower groups, expand the use range of conventional series connection differential pressure heat coupled, realized the lowest energy consumption of whole rectifying and purifying system.
(2) to be condensed to the required thermal load of the required refrigeration duty of supercooled state and the first tower bottom of rectifying tower vaporizing liquid suitable for the outer overhead vapours of Second distillation column, realizes differential pressure heat coupling, mates heat exchange.When two when tower-coupled, Energy Intensity Reduction 50%; When three when tower-coupled, Energy Intensity Reduction 75%, and the thermal source of Second distillation column adopts the heat-eliminating medium high-temperature water of reduction operation, realizes the exchange of purification process and reduction operation cooling and heating load, at utmost reduces polysilicon cost.
(3) rectifying tower tower top steam total condensation or excessively cold after the condensation of condensation reboiler, frozen-free device, has reduced facility investment, has reduced equipment configuration and pipeline configuration difficulty, expand the use range of differential pressure heat coupled, especially for the tower group of transformation project.
Embodiment
Polysilicon system comprises to be processed the topping still group of cold hydrogenation material and processes the each group of low recovery tower boiling of tower height.The inlet amount of topping still group is 60m
3/ h, feed composition is trichlorosilane 20wt%, dichloro-dihydro silicon 2wt%, silicon tetrachloride 78wt%, is entrained with the granule foreigns such as part silica flour, metallic compound, and contains a large amount of non-condensable gases such as hydrogen, hydrogenchloride in material; The inlet amount of recovery tower is 35m
3/ h, feed composition is trichlorosilane 93wt%, dichloro-dihydro silicon 3wt%, silicon tetrachloride 4wt%.
According to the coupling of routine series connection differential pressure heat, topping still group does not possess series connection differential pressure heat coupling condition.Topping still group does not possess series connection differential pressure heat coupling reason: in material, dichloro-dihydro silicon and content of silicon tetrachloride are all larger, and the granule foreign that contains cold hydrogenation material, topping still group adopts sieve-tray tower, the tower top tower base pressure of sieve-tray tower is poor larger, if adopt differential pressure heat coupling, cause column bottom temperature to exceed 120 degree, too small with the heating medium high-temperature water temperature difference, and a large amount of non-condensable gases such as hydrogen, hydrogenchloride causes tower fluctuation in cold hydrogenation material, and then affect the stability of differential pressure heat coupling.
This programme is that topping still group is first de-heavy rear de-light, first discharge a large amount of non-condensable gases by weight-removing column tower top tail gas, reduce the influence of fluctuations to follow-up tower, remove in raw material 78% silicon tetrachloride by weight-removing column, greatly reduce lightness-removing column load, and ensure that in the material of lightness-removing column be trichlorosilane more than 90wt%; Press by adjusting backflow charge ratio and tower, the lightness-removing column of the lightness-removing column of topping still group and recovery tower is adopted to the coupling of onrelevant tower differential pressure heat.
Idiographic flow is for as shown in Figure 3: hydrogenation condensation material S01 enters and slightly heats up in a steamer weight-removing column T01, overhead vapours S02 is through condenser E01 condensation, phlegma S03 enters return tank V01, phlegma S04 enters reflux pump P01, after pump, a liquid part is returned and is slightly heated up in a steamer weight-removing column T01 as phegma S05, part liquid S06 enters and slightly heats up in a steamer lightness-removing column T02, Produced Liquid S07 at the bottom of tower, according to certain ratio, a part enters reboiler E02, after reboiler heating vaporization, gas S08 returns and slightly heats up in a steamer weight-removing column T01, part Produced Liquid S09 is as raffinate extraction, silicon tetrachloride is that S10 is by side line extraction, slightly heat up in a steamer the overhead vapours S11 of lightness-removing column T02 through condenser E03 condensation, phlegma S12 enters return tank V02, phlegma S13 enters reflux pump P02, after pump, a liquid part is returned and is slightly heated up in a steamer lightness-removing column T02 as phegma S14, and a part of liquid S15 is as light constituent extraction, goes out Produced Liquid S16 at the bottom of tower, according to certain ratio, a part enters condensation reboiler E04, and after condensation reboiler heating vaporization, gas S17 returns and slightly heats up in a steamer lightness-removing column T02, and a part of Produced Liquid S18 is as product extraction, reclaimed materials S19 enters recovery tower 1 tower T03, overhead vapours S20 enters the shell side heating medium entrance of condensation reboiler E04, through condensation reboiler, condensed material S21 enters return tank V03, phlegma S22 enters reflux pump P03, after pump, a liquid part is returned to recovery tower 1 tower T03 as phegma S23, part liquid S24 extraction, Produced Liquid S25 at the bottom of extraction tower, according to certain ratio, a part enters condensation reboiler or common reboiler E05, gas S26 recovery tower 1 tower T03 after heating vaporization, part liquid S27 extraction, recovery tower 1 tower is determined flow process according to place tower group feature again, no longer describe in detail herein.
The tower top pressure of the lightness-removing column T02 of topping still is 0.25MPa, and tower top temperature is 55 DEG C, and tower top tower base pressure is poor is 0.06MPa, and tower reactor pressure and temperature is respectively 0.31MPa and 69 DEG C, and backflow charge ratio is 5.3; The tower top pressure of recovery tower 1 tower T03 is 0.65MPa, and tower top temperature is 81 DEG C, and tower top tower base pressure is poor is 0.02MPa, and tower reactor pressure and temperature is respectively 0.67MPa and 100 DEG C, and backflow charge ratio is 2.16.Concrete each tower cooling and heating load is in table 1.
Table 1
| Cooling load/M.kcal/hr | Heating load/M.kcal/hr | |
| Topping still lightness-removing column | 3.88 | 0(4.23) |
| Recovery tower 1 tower | 0（4.27） | 5.51 |
| Add up to (without coupling) | 8.15 | 10.58 |
| Add up to (thermal coupling of onrelevant tower) | 3.88 | 5.51 |
As shown in Table 1, when topping still lightness-removing column and recovery tower 1 tower are during without coupling, cooling and heating load 8.15M.kcal/hr and 10.58M.kcal/hr respectively;
When two towers adopt the coupling of onrelevant tower differential pressure heats, cooling and heating load 3.88M.kcal/hr and 5.51M.kcal/hr respectively, with compared with coupling, cooling and heating load respectively energy-conservation 52% and 48%, energy-saving effect is remarkable.
In addition, term " first ", " second " be only for describing object, and can not be interpreted as instruction or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more these features can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the present utility model, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In the utility model, unless otherwise clearly defined and limited, the terms such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and for example, can be to be fixedly connected with, and can be also to removably connect, or integral; Can be mechanical connection, can be also electrical connection; Can be to be directly connected, also can indirectly be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements.For the ordinary skill in the art, can understand as the case may be the concrete meaning of above-mentioned term in the utility model.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present utility model or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, to the schematic statement of above-mentioned term needn't for be identical embodiment or example.And, specific features, structure, material or the feature of description can one or more embodiment in office or example in suitable mode combination.In addition,, not conflicting in the situation that, those skilled in the art can carry out combination and combination by the feature of the different embodiment that describe in this specification sheets or example and different embodiment or example.
Although illustrated and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment in scope of the present utility model, amendment, replacement and modification.
Claims (2)
1. a system for onrelevant tower differential pressure heat coupling chlorine purification silane, is characterized in that, comprising:
The first rectifying tower and Second distillation column, each rectifying tower in described the first rectifying tower and Second distillation column all has the opening for feed, air outlet, liquid outlet, fluid inlet and the inlet mouth that are positioned on this rectifying tower;
The first reboiler and the second reboiler, each reboiler in described the first reboiler and the second reboiler all has and is positioned at fluid inlet, air outlet, steam inlet and condensate outlet on this reboiler,
The first reflux pump and the second reflux pump, each reflux pump in described the first reflux pump and the second reflux pump all has the import and the pump discharge that are positioned on this reflux pump;
The first return tank and the second return tank, each return tank in described the first return tank and the second return tank all has the tank import and the tank outlet that are positioned on this return tank;
A condenser, a described condenser has inlet mouth, liquid outlet, low-temperature receiver import and low-temperature receiver outlet;
Wherein,
The air outlet of described the first rectifying tower is connected with the inlet mouth of described condenser, the liquid outlet of described condenser is connected with the tank import of described the first return tank, the tank outlet of described the first return tank is connected with the pump inlet of described the first reflux pump, the pump discharge of described the first reflux pump is connected with the fluid inlet of described the first rectifying tower, to a part of chlorosilane condensate liquid is back to described the first rectifying tower;
The fluid inlet of described the first reboiler and the second reboiler is connected with the liquid outlet of described the first rectifying tower and Second distillation column respectively successively, to a part for liquid at the bottom of chlorosilane tower is heated and boiled; The air outlet of described the first reboiler and the second reboiler is connected with the inlet mouth of described the first rectifying tower and Second distillation column respectively successively;
The air outlet of described Second distillation column is connected with the steam inlet of described the first reboiler, the condensate outlet of described the first reboiler is connected with the tank import of described the second return tank, the tank outlet of described the second return tank is connected with the pump inlet of described the second reflux pump, the pump discharge of described the second reflux pump is connected with the fluid inlet of described Second distillation column, to a part for chlorosilane condensate liquid is back to described Second distillation column;
Wherein,
The low-temperature receiver import of described condenser is connected with low-temperature receiver;
The steam inlet of described the second reboiler is connected with thermal source.
2. the system of onrelevant tower differential pressure heat coupling chlorine purification silane according to claim 1, is characterized in that, the opening for feed of described the first rectifying tower and Second distillation column is connected from different chlorosilane feedwaies respectively.
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| CN201420151795.1U CN203754435U (en) | 2014-03-31 | 2014-03-31 | System of purifying chlorosilane by use of differential pressure thermal coupling of uncorrelated towers |
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| CN201420151795.1U CN203754435U (en) | 2014-03-31 | 2014-03-31 | System of purifying chlorosilane by use of differential pressure thermal coupling of uncorrelated towers |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950935A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | System for purifying chlorosilane through non-relevant tower differential pressure thermal coupling |
| CN105413221A (en) * | 2016-01-18 | 2016-03-23 | 中国恩菲工程技术有限公司 | Rectifying system |
| CN110282655A (en) * | 2019-08-08 | 2019-09-27 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
-
2014
- 2014-03-31 CN CN201420151795.1U patent/CN203754435U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950935A (en) * | 2014-03-31 | 2014-07-30 | 中国恩菲工程技术有限公司 | System for purifying chlorosilane through non-relevant tower differential pressure thermal coupling |
| CN103950935B (en) * | 2014-03-31 | 2016-03-30 | 中国恩菲工程技术有限公司 | The system of onrelevant tower differential pressure heat coupling chlorine purification silane |
| CN105413221A (en) * | 2016-01-18 | 2016-03-23 | 中国恩菲工程技术有限公司 | Rectifying system |
| CN110282655A (en) * | 2019-08-08 | 2019-09-27 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
| CN110282655B (en) * | 2019-08-08 | 2021-12-03 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectification method |
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