CN102153092B - Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane - Google Patents

Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane Download PDF

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CN102153092B
CN102153092B CN2011101078175A CN201110107817A CN102153092B CN 102153092 B CN102153092 B CN 102153092B CN 2011101078175 A CN2011101078175 A CN 2011101078175A CN 201110107817 A CN201110107817 A CN 201110107817A CN 102153092 B CN102153092 B CN 102153092B
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removing column
lightness
weight
pipeline
tower
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CN102153092A (en
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刘春江
段长春
李雪
袁希钢
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Tianjin University
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Abstract

The invention discloses a heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane. The steam at the top of a high-pressure tower which is a high-boiling-fraction removal column is used to heat liquid at the bottom of a low-pressure tower which is a low-boiling-fraction removal column, the steam at the top of the high-boiling-fraction removal column is condensed, and the process is a multi-effect distillation process; meanwhile, the steam at the top of the low-boiling-fraction removal column is subjected to pressure and temperature rise through a compressor and then is used for heating the liquid at the bottom of the high-boiling-fraction removal column, the steam at the top of the low-boiling-fraction removal column is condensed, and the process is a heat pump distillation process; and the integration of the heat pump distillation and multi-effect distillation can be realized in the whole process. In the whole process flow, one compressor is additionally arranged, the heat exchange process inside a rectification system is realized by two heat exchangers and condensers and reboilers are saved simultaneously, that is to say, small amount of electricity consumption of one compressor is added and a large amount of cold energy and heat public works are saved, and thereby the energy consumption for the whole rectification and purification process of the trichlorosilane is greatly reduced.

Description

Trichlorosilane purifying plant and technology that a kind of heat pump distillation and multiple-effect rectifying are integrated
Technical field
The invention belongs to the distillation technology field, relate to the device and the technology of heat pump distillation and multiple-effect rectifying, particularly a kind of heat pump distillation and multiple-effect rectifying integrating device and technology that is applied to the trichlorosilane purification.
Background technology
The production of polysilicon corporate boss will adopt the improvement Siemens Method at present.This method comprises five key links: synthetic, the rectification and purification of trichlorosilane of trichlorosilane, the hydrogen reduction of trichlorosilane, the recovery of tail gas and the hydrogenation of silicon tetrachloride separate.Wherein, links such as the purification of trichlorosilane, tail gas recycle separation relate to rectifying, and required distillation system has high reflux ratio and high theoretical stage characteristic, require foreign matter contents such as B, P at the PPT order of magnitude, are high energy consumption, the high pollution processes of generally acknowledging.
Heat pump distillation and multiple-effect rectifying have been widely used in the various Chemical Manufacture as two kinds of power-saving technologies that can effectively improve rectifying thermo-efficiency.Conventional rectifying tower all is to take heat away from overhead condenser, and simultaneously to tower still reboiler heat supplied, the heat that common overhead condenser is taken away is about 90% of a tower still reboiler adding heat, and the energy utilization is very unreasonable.Utilize heat pump distillation then to realize the heat transferred tower still reboiler that overhead condenser is taken away, reduced energy consumption significantly.Usually the achievement coefficient of heat pump is about 3~4, that is to say, heat pump can be sent to high temp objects from cryogenic object with 3 to 4 times heat energy of self institute's energy requirement, and the higher heat pump achievement coefficient of performance can reach 6~8.Multiple-effect rectifying is that rectifying tower is divided into can the different multitower in position, can the position than the top steam of high tower to reboiler heat supply that can the low tower in position, it is condensed itself simultaneously.Like this, just the tower still of first tower need add heat in multiple-effect rectifying, and the overhead vapours of last tower carries out condensation with heat-eliminating medium, and all the other each towers then no longer need the external world and carry out heat supply and cooling, so it has very remarkable energy saving effect.Theoretically, compare with single tower, the energy-saving effect of the double-effect rectification of being made up of double tower is 50%, and the energy-saving effect of three-effect rectification is 67%.
In recent years, along with polysilicon becomes the strategic industry that country first develops gradually, the trichlorosilane rectification and purification technology of improving in the production of polysilicon technology made its energy-saving and cost-reducing task increasingly important and urgent.At present, this field is to very shortage of the introduction of heat pump distillation and multiple-effect distillation technology, and the technology that heat pump distillation and multiple-effect rectifying is integrated is blank especially then.
Summary of the invention
Trichlorosilane purifying plant and technology that a kind of heat pump distillation of the present invention and multiple-effect rectifying are integrated; Purpose is to overcome existing installation and technological above-mentioned shortcoming; A kind of heat pump distillation and integrated device and technology of multiple-effect rectifying that trichlorosilane is purified that is used for is provided, adopts this technology can reduce the energy consumption in the trichlorosilane rectification and purification process greatly.
The present invention realizes through following technical scheme:
Trichlorosilane purifying plant and technology that a kind of heat pump distillation of the present invention and multiple-effect rectifying are integrated; Respectively heat pump distillation (as shown in Figure 1) and multiple-effect rectifying (as shown in Figure 2) are applied to the trichlorosilane rectifying; And the two is combined (as shown in Figure 3) be used, further reach energy-saving and cost-reducing effect.This technical process comprises two or three rectifying tower, a compressor, two or three interchanger and some material pipelines etc.With the tower bottoms body heat exchange of the overhead vapours and the lower pressure column of high-pressure tower, simultaneously with the overhead vapours of lower pressure column through the thermal-pump unit tower bottoms body heat exchange of back and high-pressure tower of heating up of boosting, like this each heated while of Tata still liquid, overhead vapours also is condensed.Whole process flow has just increased by a compressor and has utilized two to three interchanger to realize the thermal exchange process that distillation system is inner; But all condensing surfaces and reboiler have been saved; It is a small amount of power consumption that has just increased by a compressor in the process; And practiced thrift a large amount of colds and heat general facilities, thereby make the rectification and purification process of whole trichlorosilane greatly reduce energy consumption.
The trichlorosilane purifying plant that a kind of heat pump distillation of the present invention and multiple-effect rectifying are integrated comprises lightness-removing column, weight-removing column, compressor, interchanger and material pipeline; The integrating device that it is characterized in that heat pump distillation and double-effect rectification or three-effect rectification.
The integrated technique of heat pump distillation and double-effect rectification, with the tower bottoms body heat exchange of the overhead vapours and the lightness-removing column 1 of weight-removing column 2, simultaneously with the overhead vapours of lightness-removing column 1 through the thermal-pump unit 7 tower bottoms body heat exchange of back and weight-removing column 2 of heating up of boosting.
As shown in Figure 3, opening for feed is established at lightness-removing column 1 middle part, and one of discharging pipeline returns lightness-removing column 1 inner bottom part after heating up through interchanger I 4 at the bottom of the tower, and the middle part of another Guan Jingyu weight-removing column 2 connects the charging as weight-removing column; Lightness-removing column 1 cat head discharging pipeline passes through interchanger II 5 and discharging pipeline heat exchange at the bottom of weight-removing column 2 towers earlier again after compressor 7 boosts intensification, a pipeline returns the backflow of lightness-removing column 1 inner top afterwards, and another pipeline is treaded; As charging, the discharging pipeline returns weight-removing column 2 tower stills with the lightness-removing column 1 overhead vapours pipeline after interchanger II 5 heat exchange that boosts after heating up through compressor 7 to weight-removing column 2 at the bottom of weight-removing column 2 towers with lightness-removing column 1 tower still extraction liquid, and another pipeline is treaded; Weight-removing column 2 overhead vapours pipeline after interchanger I 4 and lightness-removing column 1 tower bottoms body heat exchange returns weight-removing column 2 trim the top of column, and another pipeline is treaded high-purity trichlorosilane.
The integrated technique of heat pump distillation and three-effect rectification; Tower bottoms body heat exchange with the overhead vapours and the lightness-removing column 1 of weight-removing column 2; The tower bottoms body heat exchange of the overhead vapours of secondary lightness-removing column 3 and weight-removing column 2, simultaneously with the overhead vapours of lightness-removing column 1 through the thermal-pump unit 7 tower bottoms body heat exchange of back and secondary lightness-removing column 3 of heating up of boosting.
As shown in Figure 4; Opening for feed is established at lightness-removing column 1 middle part, and overhead vapours heats the effusive liquid of secondary lightness-removing column 3 tower stills through interchanger III6 after compressor 7 boosts intensification, after lightness-removing column 1 overhead vapours is condensed simultaneously; Article one, pipeline returns the lightness-removing column top and refluxes another pipeline extraction; Pipeline of the effusive liquid of lightness-removing column 1 tower still returns lightness-removing column 1 bottom after being heated by the overhead vapours of weight-removing column 2, and another pipeline is connected to the charging of weight-removing column 2 middle parts as weight-removing column 2; Be condensed after the tower bottoms body heat exchange of the overhead vapours of weight-removing column 2 and lightness-removing column 1; Article one, pipeline returns the top backflow of weight-removing column 2; Another is connected to the charging of the middle part of secondary lightness-removing column 3 as secondary lightness-removing column 3 towers; Pipeline of the effusive liquid of weight-removing column 2 tower stills returns weight-removing column 2 bottoms, another extraction after being heated in interchanger II 5 by the overhead vapours of secondary lightness-removing column 3; The overhead vapours of secondary lightness-removing column 3 is returned cat head by pipeline after the effusive condenses of weight-removing column 2 tower stills and goes into to reflux in interchanger II 5; Another pipeline is connected on the feeding line of lightness-removing column 1 and proceeds rectifying; Pipeline of the effusive liquid of secondary lightness-removing column 3 tower stills returns secondary lightness-removing column 3 bottoms after being heated by the overhead vapours of the lightness-removing column 1 of the intensification of being boosted through compressor 7, and another pipeline is the high-purity trichlorosilane of extraction then; The tower bottoms body of the overhead vapours heating lightness-removing column 1 of weight-removing column 2, the overhead vapours of weight-removing column 2 is cooled simultaneously, the tower bottoms body of the overhead vapours heating weight-removing column 2 of secondary lightness-removing column 3, the overhead vapours of secondary lightness-removing column 3 is cooled simultaneously.
Heat pump distillation and integrated device and the technology of multiple-effect rectifying have been the invention is characterized in to the purification applications of trichlorosilane; Utilizing high-pressure tower is that the overhead vapours of weight-removing column heats the tower bottoms body that lower pressure column is a lightness-removing column; And the weight-removing column overhead vapours is condensed, and this process is the multiple-effect rectifying; Again the overhead vapours of lightness-removing column is boosted through compressor simultaneously and remove to heat the tower bottoms body of weight-removing column after heating up, and the lightness-removing column overhead vapours is condensed, this process is the heat pump distillation process; Whole process has realized the integrated of heat pump distillation and multiple-effect rectifying, and whole process flow has just increased by a compressor and utilize two interchanger to realize the thermal exchange process that distillation system is inner, but has saved all condensing surfaces and reboiler.
Effect of the present invention and advantage be, utilizes the process of integrated device of heat pump distillation and multiple-effect rectifying and technology purification rectifying trichlorosilane not need condensing surface and reboiler, saved a large amount of colds and heat general facilities; Just increase a small amount of power consumption of a compressor in the process, thereby made the rectification and purification process of whole trichlorosilane greatly reduce energy consumption.
Description of drawings
Fig. 1 is heat pump distillation apparatus and process schematic representation;
Fig. 2 is multiple-effect rectifier unit and process schematic representation;
Fig. 3 is heat pump distillation of the present invention and double-effect rectification integrated trichlorosilane purification rectifier unit and process schematic representation;
Fig. 4 is heat pump distillation of the present invention and three-effect rectification integrated trichlorosilane purification rectifier unit and process schematic representation;
Fig. 5 is existing trichlorosilane purification rectifier unit and process schematic representation;
Wherein, 1-lightness-removing column, 2-weight-removing column, 3-secondary lightness-removing column, 4-interchanger I, 5-interchanger II, 6-interchanger III, 7-compressor, 8-reboiler I, 9-reboiler II, 10-condensing surface I, 11-condensing surface II.
Embodiment
According to accompanying drawing the present invention is done further detailed description below:
Trichlorosilane purifying plant and technology that heat pump distillation of the present invention and multiple-effect rectifying are integrated; Respectively heat pump distillation (as shown in Figure 1) and multiple-effect rectifying (as shown in Figure 2) are applied to the trichlorosilane rectifying; And the two is combined (as shown in Figure 3) be used, further reach energy-saving and cost-reducing effect.This technical process comprises two or three rectifying tower, a compressor, two or three interchanger and some material pipelines etc.In this rectifying, utilizing high-pressure tower is that the overhead vapours of weight-removing column heats the tower bottoms body that lower pressure column is a lightness-removing column, and high-pressure tower to be the weight-removing column overhead vapours be condensed, realize the multiple-effect rectifying; Again the overhead vapours of lightness-removing column is boosted through compressor simultaneously and remove to heat the tower bottoms body of weight-removing column after heating up, and the lightness-removing column overhead vapours is condensed, and realizes the heat pump distillation process, whole process has realized the integrated of heat pump distillation and multiple-effect rectifying.Utilize the technology of the integrated technology purification rectifying trichlorosilane of heat pump distillation and multiple-effect rectifying; Compare with existing distillation system; Technical process has just increased a compressor and has utilized two to three interchanger to realize the thermal exchange process that distillation system is inner; But whole process does not need condensing surface and reboiler, has promptly just increased a small amount of power consumption, thereby but has saved a large amount of colds and the heat general facilities makes the rectification and purification process energy consumption of trichlorosilane reduce greatly.
Embodiment 1: as shown in Figure 3, integrated production equipment and the technical process thereof that comes purify trichlorosilane of heat pump distillation and double-effect rectification comprises lightness-removing column 1, weight-removing column 2, compressor 7, interchanger I 4, interchanger II 5 and some material pipelines etc.Opening for feed is established at lightness-removing column 1 middle part, and one of discharging pipeline returns lightness-removing column 1 inner bottom part after heating up through interchanger I 4 at the bottom of the tower, and the middle part of another Guan Jingyu weight-removing column 2 connects the charging as weight-removing column; Lightness-removing column 1 cat head discharging pipeline passes through interchanger II 5 and discharging pipeline heat exchange at the bottom of weight-removing column 2 towers earlier again after compressor 7 boosts intensification, a pipeline returns the backflow of lightness-removing column 1 inner top afterwards, and another pipeline is treaded, and this process is the heat pump distillation process; As charging, the discharging pipeline returns weight-removing column 2 tower stills with the lightness-removing column 1 overhead vapours pipeline after interchanger II 5 heat exchange that boosts after heating up through compressor 7 to weight-removing column 2 at the bottom of weight-removing column 2 towers with lightness-removing column 1 tower still extraction liquid, and another pipeline is treaded; Weight-removing column 2 overhead vapours pipeline after interchanger I 4 and lightness-removing column 1 tower bottoms body heat exchange returns weight-removing column 2 trim the top of column; Another pipeline is treaded high-purity trichlorosilane; This process is the double-effect rectification process, and whole process has realized the integrated of heat pump distillation and multiple-effect rectifying.Compare with conventional process flow shown in Figure 5, heat pump distillation and the integrated technology of multiple-effect rectifying have been saved 8,9 and two condensing surfaces 10,11 of two reboilers, have saved great amount of heat and cold general facilities, and have just increased a small amount of power consumption of compressor.Usually the achievement coefficient of heat pump is about 3~4, that is to say, heat pump can be sent to high temp objects from cryogenic object with 3 to 4 times heat energy of self institute's energy requirement, and the higher heat pump achievement coefficient of performance can reach 6~8.Simultaneously, double-effect rectification is also energy-conservation 50% than single tower distillation theoretical value, visiblely utilizes the heat pump distillation of the present invention and the technology of the integrated purify trichlorosilane of multiple-effect rectifying to greatly reduce energy consumption than traditional trichlorosilane rectification process.
The purifying plant of existing trichlorosilane and technology; Lightness-removing column, weight-removing column all are equipped with condensing surface and reboiler separately; Promptly be provided with two condensing surfaces and two reboilers altogether, the general facilities energy consumption of condensing surface and reboiler is 1000KW, and then trichlorosilane distillation system total energy consumption is 4000KW; And under the same process condition, in the trichlorosilane purifying plant and technology that heat pump distillation and double-effect rectification are integrated, be a compressor energy consumption 300KW.It is thus clear that utilize the heat pump distillation of the present invention and the technology of the integrated purify trichlorosilane of multiple-effect rectifying to greatly reduce energy consumption than traditional trichlorosilane rectification process.
Embodiment 2: as shown in Figure 4; Integrated technology and the production equipment thereof that comes purify trichlorosilane of heat pump distillation and three-effect rectification comprises lightness-removing column 1, weight-removing column 2, secondary lightness-removing column 3, compressor 7, interchanger I 4, interchanger II 5, interchanger III 6 and some material pipelines.Three pressure tower levels wherein, secondary lightness-removing column 3 is the highest, and weight-removing column 2 takes second place, and lightness-removing column 1 is minimum.Opening for feed is established at lightness-removing column 1 middle part; Overhead vapours heats the effusive liquid of secondary lightness-removing column 3 tower stills through interchanger III 6 after compressor 7 boosts intensification; After lightness-removing column 1 overhead vapours is condensed simultaneously; Article one, pipeline returns the backflow of lightness-removing column top, another pipeline extraction, and this process has realized the heat pump distillation process; Pipeline of the effusive liquid of lightness-removing column 1 tower still returns lightness-removing column 1 bottom after being heated by the overhead vapours of weight-removing column 2, and another pipeline is connected to the charging of weight-removing column 2 middle parts as weight-removing column 2; Be condensed after the tower bottoms body heat exchange of the overhead vapours of weight-removing column 2 and lightness-removing column 1; Article one, pipeline returns the top backflow of weight-removing column 2; Another is connected to the charging of the middle part of secondary lightness-removing column 3 as secondary lightness-removing column 3 towers; Pipeline of the effusive liquid of weight-removing column 2 tower stills returns weight-removing column 2 bottoms, another extraction after being heated in interchanger II 5 by the overhead vapours of secondary lightness-removing column 3; The overhead vapours of secondary lightness-removing column 3 is refluxed by the top that pipeline after the effusive condenses of weight-removing column 2 tower stills returns secondary lightness-removing column 3 in interchanger II 5; Another pipeline is connected on the feeding line of lightness-removing column 1 and proceeds rectifying; Pipeline of the effusive liquid of secondary lightness-removing column 3 tower stills returns secondary lightness-removing column 3 bottoms after being heated by the overhead vapours of the lightness-removing column 1 of the intensification of being boosted through compressor 7, and another pipeline is the high-purity trichlorosilane of extraction then; The tower bottoms body of the overhead vapours heating lightness-removing column 1 of weight-removing column 2; The overhead vapours of weight-removing column 2 is cooled simultaneously; The tower bottoms body of the overhead vapours heating weight-removing column 2 of secondary lightness-removing column 3; The overhead vapours of secondary lightness-removing column 3 is cooled simultaneously, has realized the three-effect rectification process, and whole process has realized the integrated of heat pump distillation and multiple-effect rectifying.
Compare with existing trichlorosilane purifying plant and technology; Lightness-removing column, weight-removing column, secondary lightness-removing column three towers all are equipped with separately condensing surface and reboiler; Promptly be provided with three condensing surfaces and three reboilers altogether; The general facilities energy consumption of condensing surface and reboiler is 1000KW, and then trichlorosilane distillation system total energy consumption is 6000KW; And under the same process condition, in the trichlorosilane purifying plant and technology that heat pump distillation and three-effect rectification are integrated, just a compressor energy consumption 300KW is about 1/20 of former energy consumption.It is thus clear that utilize the heat pump distillation of the present invention and the technology of the integrated purify trichlorosilane of multiple-effect rectifying to greatly reduce energy consumption than traditional trichlorosilane rectification process.
The integrated device technique of heat pump distillation and multiple-effect rectifying not only can be used for the rectification and purification process of trichlorosilane, can also be used in the rectifyinges such as tail gas recycle separation of polysilicon production process.Adopt this technology, can reduce the energy consumption in the trichlorosilane rectification and purification engineering greatly, thereby reduced the energy consumption of polysilicon production process.

Claims (2)

1. heat pump distillation and the integrated trichlorosilane purifying plant of double-effect rectification comprise lightness-removing column, weight-removing column, compressor, interchanger and material pipeline; It is characterized in that tower bottoms body heat exchange with the overhead vapours and the lightness-removing column (1) of weight-removing column (2), simultaneously with the overhead vapours of lightness-removing column (1) through compressor (7) the tower bottoms body heat exchange of back and weight-removing column (2) of heating up of boosting; Opening for feed is established at lightness-removing column (1) middle part, and one of discharging pipeline returns bottom the lightness-removing column (1) after heating up through interchanger I (4) at the bottom of the tower, and another middle part with weight-removing column (2) is connected the charging as weight-removing column (2); Lightness-removing column (1) cat head discharging pipeline passes through interchanger II (5) and discharging pipeline heat exchange at the bottom of weight-removing column (2) tower earlier again after compressor (7) boosts intensification, a pipeline returns lightness-removing column (1) top and refluxes another pipeline extraction afterwards; Weight-removing column (2) with lightness-removing column (1) tower still extraction liquid as charging; The discharging pipeline returns weight-removing column (2) tower still, another pipeline extraction with lightness-removing column (1) the overhead vapours pipeline after interchanger II (5) heat exchange that boosts after heating up through compressor (7) at the bottom of weight-removing column (2) tower; Weight-removing column (2) overhead vapours pipeline after interchanger I (4) and the heat exchange of lightness-removing column (1) tower bottoms body returns weight-removing column (2) trim the top of column, the high-purity trichlorosilane of another pipeline extraction.
2. heat pump distillation and the integrated trichlorosilane purifying plant of three-effect rectification comprise lightness-removing column, weight-removing column, compressor, interchanger and material pipeline; It is characterized in that tower bottoms body heat exchange with the overhead vapours and the lightness-removing column (1) of weight-removing column (2); The tower bottoms body heat exchange of the overhead vapours of secondary lightness-removing column (3) and weight-removing column (2), simultaneously with the overhead vapours of lightness-removing column (1) through compressor (7) the tower bottoms body heat exchange of back and secondary lightness-removing column (3) of heating up of boosting; Opening for feed is established at lightness-removing column (1) middle part; Overhead vapours heats the effusive liquid of secondary lightness-removing column (3) tower still through interchanger III (6) after compressor (7) boosts intensification; After lightness-removing column (1) overhead vapours is condensed simultaneously; Article one, pipeline returns the lightness-removing column top and refluxes another pipeline extraction; Pipeline of the effusive liquid of lightness-removing column (1) tower still returns lightness-removing column (1) bottom after being heated by the overhead vapours of weight-removing column (2), and another pipeline is connected to the charging of weight-removing column (2) middle part as weight-removing column (2); Be condensed after the tower bottoms body heat exchange of the overhead vapours of weight-removing column (2) and lightness-removing column (1); Article one, pipeline returns the top backflow of weight-removing column (2); Another is connected to the charging of the middle part of secondary lightness-removing column (3) as secondary lightness-removing column (3) tower; After being heated in interchanger II (5) by the overhead vapours of secondary lightness-removing column (3), pipeline of the effusive liquid of weight-removing column (2) tower still returns weight-removing column (2) bottom, another pipeline extraction; The overhead vapours of secondary lightness-removing column (3) is returned trim the top of column by pipeline after the effusive condenses of weight-removing column (2) tower still in interchanger II (5); Another pipeline is connected on the feeding line of lightness-removing column (1) and proceeds rectifying; Pipeline of the effusive liquid of secondary lightness-removing column (3) tower still returns secondary lightness-removing column (3) bottom after being heated by the overhead vapours of the lightness-removing column (1) of the intensification of being boosted through compressor (7), and another pipeline is the high-purity trichlorosilane of extraction then.
CN2011101078175A 2011-04-27 2011-04-27 Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane Expired - Fee Related CN102153092B (en)

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CN102649019B (en) * 2012-04-17 2014-10-22 中国恩菲工程技术有限公司 Trichlorosilane rectification system
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CN104071791B (en) * 2014-07-11 2016-08-24 中国恩菲工程技术有限公司 The method of purification of trichlorosilane
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