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CN209411790U - A kind of Finestill energy-saving apparatus purified for restoring chlorosilane - Google Patents

A kind of Finestill energy-saving apparatus purified for restoring chlorosilane Download PDF

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Publication number
CN209411790U
CN209411790U CN201822177720.1U CN201822177720U CN209411790U CN 209411790 U CN209411790 U CN 209411790U CN 201822177720 U CN201822177720 U CN 201822177720U CN 209411790 U CN209411790 U CN 209411790U
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China
Prior art keywords
distillation column
reboiler
pipeline connection
tower
outlet
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Expired - Fee Related
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CN201822177720.1U
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Chinese (zh)
Inventor
晋正茂
董燕军
武振国
李天客
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INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd
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INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The utility model discloses a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, including liquid-phase reduction chlorosilane storage tank, first rectifying column, Second distillation column, third distillation column, the first reboiler, the first tower reactor pump, the second return tank, the first reflux pump, the second reflux pump, third reboiler, third condenser, third return tank, third reflux pump, third tower reactor pump;The discharge port of liquid-phase reduction chlorosilane storage tank is connected to the feed inlet of first rectifying column by delivery pump, the cold medium entrance of first rectifying column tower reactor liquid outlet and the first reboiler passes through pipeline connection, the outlet of first reboiler cold medium passes through pipeline connection with first rectifying column air inlet, the thermal medium entrance and heat source of first reboiler pass through pipeline connection, the utility model realizes production of polysilicon closed cycle, thus, heat, which rationally utilizes, to be accomplished to the Finestill energy-saving apparatus of reduction chlorosilane purification, save considerably energy consumption, resource, good economical benefit are saved.

Description

A kind of Finestill energy-saving apparatus purified for restoring chlorosilane
Technical field:
It is the utility model relates to the technical field of chlorosilane purification, in particular to a kind of for restoring the essence of chlorosilane purification Evaporate energy saver.
Background technique:
Polysilicon is a kind of superelevation pure material, is used for integrated circuit, electronic device and solar battery, be human society into The fields such as step, each department of national economy and defense technology equipment are indispensable and the most important functional material and basic material of substitution Material, the production technology of polysilicon are mainly improved Siemens and silane thermal decomposition process, and the main production process of current country's polysilicon is Improved Siemens.Siemens Method is that column of polysilicon is produced by way of vapor deposition, in order to improve raw material availability and It is environmental-friendly, on the basis of the former use closed loop production technology, that is, improved Siemens, the technique by industrial silica fume with HCl reaction, is processed into SiHCI3, then allow SiHCl3In H2Reduction deposition obtains polysilicon, reduction furnace discharge in the reduction furnace of atmosphere Tail gas H2、SiHCl3、SiCl4、SiH2Cl2Enter exhaust gas recovery system with HCl, the recycling after separation.Pass through tail After the processing of gas disposal process, the liquid phase material condensed out is known as restoring chlorosilane, is transported to rectification working process and carries out separating-purifying, High-purity refining trichlorosilane is obtained after separating by rectifying column, is transported to reduction process and is continued to use.
Conventional rectification technique is used to carry out the purification of reduction chlorosilane for two tower series connection, two towers have been respectively coupled again Device and condenser are boiled, needing to consume more steam (or hot water) and the rectifying column of recirculated water, especially first will realize SiH2Cl2、SiHCl3、SiCl4Separation, rectifying column overall height is higher, and the number of plates is more, energy consumption is larger, once invests huge. The energy consumption of purification process is one of main energy consumption of polysilicon system, therefore the energy consumption for reducing purification process is to reduce polysilicon life One of the most effective approach for producing cost, solves the problems, such as that energy consumption is high in production of polysilicon purification process, further promotes polysilicon Industry reach energy conservation, consumption reduction, safe and environment-friendly target it is increasingly important with it is urgent.
Utility model content:
The purpose of this utility model is to provide one kind to economize on resources, and good economical benefit is used to restore what chlorosilane purified Finestill energy-saving apparatus.
The utility model is implemented by following technical solution: it is a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, Including liquid-phase reduction chlorosilane storage tank, first rectifying column, Second distillation column, third distillation column, the first reboiler, the first tower reactor Pump, the reflux of the second return tank, the first reflux pump, the second reflux pump, third reboiler, third condenser, third return tank, third Pump, third tower reactor pump;The discharge port of the liquid-phase reduction chlorosilane storage tank and the feed inlet of the first rectifying column pass through conveying The cold medium entrance of pump connection, the first rectifying column tower reactor liquid outlet and first reboiler is described by pipeline connection The outlet of first reboiler cold medium passes through pipeline connection, the thermal medium of first reboiler with the first rectifying column air inlet By pipeline connection, the feed inlet of the first rectifying column tower reactor outlet and silicon tetrachloride storage tank passes through described for entrance and heat source The pump connection of one tower reactor, the gas outlet of the first rectifying column tower top and the air inlet of the Second distillation column pass through pipeline connection,
The Second distillation column tower reactor liquid outlet and the refluxing opening of the first rectifying column are connected by first reflux pump Logical, the thermal medium entrance of the Second distillation column tower top outlet and the third reboiler is by pipeline connection, and the third is again Boil the thermal medium outlet of device and the entrance of second return tank by pipeline connection, the outlet of second return tank with it is described The refluxing opening of Second distillation column is connected to by second reflux pump, and the discharge port of second reflux pump is also smart with the third The feed inlet for evaporating tower passes through pipeline connection,
The cold medium entrance of third distillation column tower reactor outlet and the third reboiler is by pipeline connection, and described the By pipeline connection, the third distillation column tower reactor goes out for the cold medium outlet of three reboilers and the air inlet of the third distillation column Material mouth is connected to secondary trichlorosilane reservoir inlet port by third tower reactor pump, third distillation column tower top gas outlet and institute The air inlet for stating third condenser passes through pipeline connection, the condensate outlet of the third condenser and the third return tank Entrance passes through pipeline connection by pipeline connection, the cold source import of the third condenser and cold source, the third return tank Outlet be connected to the refluxing opening of the third distillation column by the third reflux pump, the discharge port of the third reflux pump also with Refining trichlorosilane reservoir inlet port passes through pipeline connection.
Further, the first rectifying column and the Second distillation column are plate column.
Further, the third distillation column is packed tower.
Further, the first rectifying column tower top pressure is 0.28~0.35MPa, the first rectifying column tower top temperature 90~98 DEG C, the first rectifying column tower reactor pressure be 0.35~0.40MPa, the first rectifying column bottom temperature be 112~ 117℃。
Further, the Second distillation column tower top pressure is 0.20~0.29MPa, the Second distillation column tower top temperature 66~75 DEG C, the Second distillation column tower reactor pressure is 0.27~0.34MPa, and the Second distillation column bottom temperature is 88~95 ℃。
Further, the third distillation column tower top pressure is 0.06~0.14MPa, the third distillation column tower top temperature 44~58 DEG C, the third distillation column tower reactor pressure is 0.08~0.15MPa, the third distillation column bottom temperature 51~60 ℃。
Further, the heat source that first reboiler uses is that polycrystalline silicon device restores thermogenetic low pressure steaming more than process Vapour, the low-pressure steam pressure are 0.17~0.22MPa, and the low-pressure steam temperature is 130~136 DEG C.
Further, the cold source that the third condenser uses is recirculated water, and circulating water temperature is 22~25 DEG C.
The advantages of the utility model: (1) conventional multi-crystalline silicon is produced into purification process first rectifying column two series connection Rectifying column replacement, significantly reduce the overall height of rectifying column, greatly reduce the overall investment of equipment, reduce people The danger coefficient of work installation, maintenance;(2) the utility model adds Second distillation column tower top tail gas as the heat source of third reboiler The material of hot third distillation column tower reactor forms the pipeline of the recyclable recycling heat of steam, reduces the investment of reboiler, with biography Two tower process of uniting are compared, and can be saved steam about 40~50%, can be saved recirculated water 40~50%, solve in polysilicon system and mention The problem of pure process high energy consumption, reduce enterprise's production cost;(3) the utility model realizes production of polysilicon closed cycle, Heat, which rationally utilizes, to be accomplished to the Finestill energy-saving apparatus of reduction chlorosilane purification as a result, energy consumption is saved considerably, has saved money Source, good economical benefit have reached the zero-emission of chlorosilane tail gas, harmless treatment, have protected environment.
Detailed description of the invention:
Fig. 1 is the overall structure diagram of the utility model.
Wherein: first rectifying column 1, Second distillation column 2, third distillation column 3, the first reboiler 4, the first tower reactor pump 5, second Return tank 6, the first reflux pump 7, the second reflux pump 8, third reboiler 9, third condenser 10, third return tank 11, third are returned Stream pump 12, third tower reactor pump 13, delivery pump 14, liquid-phase reduction chlorosilane storage tank 15, silicon tetrachloride storage tank 16, refining trichlorosilane Storage tank 17, secondary trichlorosilane storage tank 18, heat source 19.
Specific embodiment:
As shown in Figure 1, a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification comprising the storage of liquid-phase reduction chlorosilane Slot 15, first rectifying column 1, Second distillation column 2, third distillation column 3, the first reboiler 4, the first tower reactor pump the 5, second return tank 6, First reflux pump 7, the second reflux pump 8, third reboiler 9, third condenser 10, third return tank 11, third reflux pump 12, Three tower reactors pump 13.
The discharge port of liquid-phase reduction chlorosilane storage tank 15 is connected to the feed inlet of first rectifying column 1 by delivery pump 14, the The cold medium entrance of one rectifying column, 1 tower reactor liquid outlet and the first reboiler 4 is gone out by pipeline connection, 4 cold medium of the first reboiler With 1 air inlet of first rectifying column by pipeline connection, the thermal medium entrance and heat source 19 of the first reboiler 4 pass through pipeline and connect mouth Logical, the heat source 19 that the first reboiler 4 uses is that polycrystalline silicon device restores thermogenetic low-pressure steam more than process, low-pressure steam pressure For 0.17~0.22MPa, low-pressure steam temperature is 130~136 DEG C, the outlet of 1 tower reactor of first rectifying column and silicon tetrachloride storage tank 16 Feed inlet by the first tower reactor pump 5 connection, the gas outlet of 1 tower top of first rectifying column and the air inlet of Second distillation column 2 pass through Pipeline connection, first rectifying column 1 are plate column, and 1 tower top pressure of first rectifying column is 0.28~0.35MPa, 1 tower of first rectifying column Top 90~98 DEG C of temperature, 1 tower reactor pressure of first rectifying column be 0.35~0.40MPa, 1 bottom temperature of first rectifying column be 112~ 117℃。
2 tower reactor liquid outlet of Second distillation column is connected to the refluxing opening of first rectifying column 1 by the first reflux pump 7, in order to have Effect saves energy, and 2 tower top outlet of Second distillation column and the thermal medium entrance of third reboiler 9 pass through pipeline connection, and third is boiled again The entrance of the thermal medium outlet of device 9 and the second return tank 6 passes through pipeline connection, the outlet of the second return tank 6 and Second distillation column 2 Refluxing opening be connected to by the second reflux pump 8, feed inlet of the discharge port of the second reflux pump 8 also with third distillation column 3 pass through pipe Road connection, Second distillation column 2 are plate column, and 2 tower top pressure of Second distillation column is 0.20~0.29MPa, 2 tower top of Second distillation column 66~75 DEG C of temperature, 2 tower reactor pressure of Second distillation column is 0.27~0.34MPa, and 2 bottom temperature of Second distillation column is 88~95 ℃。
The outlet of 3 tower reactor of third distillation column and the cold medium entrance of third reboiler 9 pass through pipeline connection, third reboiler 9 Cold medium outlet pass through pipeline connection, 3 tower reactor discharge port of third distillation column and second level trichlorine with the air inlet of third distillation column 3 18 entrance of hydrogen silicon storage tank passes through 13 connection of third tower reactor pump, the air inlet of third distillation column 3 tower top gas outlet and third condenser 10 Mouth passes through pipeline connection, third by pipeline connection, the condensate outlet of third condenser 10 and the entrance of third return tank 11 By pipeline connection, the cold source that third condenser 10 uses is recirculated water, circulating water temperature for the cold source import of condenser 10 and cold source Degree is 22~25 DEG C, and the outlet of third return tank 11 is connected to the refluxing opening of third distillation column 3 by third reflux pump 12, third For the discharge port of reflux pump 12 also with 17 entrance of refining trichlorosilane storage tank by pipeline connection, third distillation column 3 is packed tower, the Three rectifying columns, 3 tower top pressure is 0.06~0.14MPa, 44~58 DEG C of 3 tower top temperature of third distillation column, 3 tower reactor of third distillation column Pressure is 0.08~0.15MPa, 51~60 DEG C of 3 bottom temperature of third distillation column.
Because the heat source 19 that the first reboiler 4 uses is that polycrystalline silicon device restores thermogenetic low-pressure steam more than process, Temperature is 130~136 DEG C, and to improve rectification efficiency, 1 bottom temperature of first rectifying column is otherwise warm in principle no more than 120 DEG C Source 19 and bottom temperature difference are too small, it will and cause reboiler area too big, so that equipment purchase is costly, but due to first Rectifying column 1 is connected with Second distillation column 2, and too low 2 tower top pressure of Second distillation column that will lead to of 1 kettle temperature degree of first rectifying column is low, right Answer tower top temperature relatively low, so that 9 heat exchange area of third reboiler is too big;In order to guarantee that 9 heat exchange area of third reboiler is suitable, The temperature difference that need to be controlled between 3 kettle temperature degree of third distillation column and 2 tower top temperature of Second distillation column is preferably not less than 15 DEG C;Third condenser 10 are cooled down using recirculated water, and to reduce cold source load, third distillation column 3 pushes up on temperature and recirculated water water temperature difference not in principle Lower than 15 DEG C, 51~60 DEG C of 3 bottom temperature of third distillation column, in order to improve 3 tower top temperature of third distillation column, third distillation column 3 Regular silk screen packed tower is selected, so as to be substantially reduced tower top and tower reactor pressure difference, improves 3 tower top temperature of third distillation column.
Process flow is as follows: raw material initially enters first rectifying column 1, and kettle material is heated gas by the first reboiler 4 Change, so that gaseous phase materials silicon tetrachloride, trichlorosilane and dichlorosilane is risen to tower tray, with four chlorination of liquid phase material on tower tray Silicon, trichlorosilane and dichlorosilane carry out heat and mass, realize the separating-purifying of material, are realized also by first rectifying column 1 The initial gross separation of former chlorosilane material, 1 tower reactor of first rectifying column produces the silicon tetrachloride that purity is 99wt% or more, into tetrachloro SiClx storage tank 16, the gaseous products main component of 1 overhead extraction of first rectifying column be silicon tetrachloride (content be 10~15wt%), Trichlorosilane (content is 81~88%), dichlorosilane (content is 2~4wt%), the gas phase of 1 overhead extraction of first rectifying column Product enters the further separating-purifying of Second distillation column 2 by pipeline.
2 top gaseous phase product main component of Second distillation column is trichlorosilane (content is 94~97wt%) and dichloro-dihydro Silicon (content is 3~6wt%), for effectively save energy, the top gaseous phase product of Second distillation column 2 enters third as heat source 3 reboiler of rectifying column is condensed into liquid phase back to 2 return tank of Second distillation column, in 2 return tank of Second distillation column after exchanging heat Material a part enters Second distillation column 2 as phegma, and another part enters third distillation column 3 as intermediate products, makees For the charging of third distillation column 3, which is trichlorosilane (content is 94~97wt%), dichlorosilane (content is 3~6wt%), 2 tower reactor liquid phase material of Second distillation column returns to first rectifying column 1 as phegma by pipeline.
3 top gaseous phase product component of third distillation column is that (content (contains trichlorosilane for 93~96wt%), dichlorosilane Amount is 4~7wt%), 3 overhead extraction of third distillation column enters third condenser 10, enters third return tank after being condensed into liquid phase 11, liquid phase material a part returns to third distillation column 3 as phegma in third return tank 11, and a part is used as product purification three Chlorine hydrogen silicon is transported to refining trichlorosilane storage tank 17, then is transported to reduction process by pump and uses, the extraction of 3 tower reactor of third distillation column Trichlorosilane is delivered to secondary trichlorosilane storage tank 18 by third tower reactor pump 13 as secondary trichlorosilane, then using height Boiling system carries out further purification processes.
The above is only the preferred embodiments of the present utility model only, is not intended to limit the utility model, all practical at this Within novel spirit and principle, any modification, equivalent replacement, improvement and so on should be included in the guarantor of the utility model Within the scope of shield.

Claims (8)

1. a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that it includes the storage of liquid-phase reduction chlorosilane Slot, first rectifying column, Second distillation column, third distillation column, the first reboiler, the first tower reactor pump, the second return tank, the first reflux Pump, the second reflux pump, third reboiler, third condenser, third return tank, third reflux pump, third tower reactor pump;The liquid phase The discharge port of reduction chlorosilane storage tank is connected to the feed inlet of the first rectifying column by delivery pump, the first rectifying column tower The cold medium entrance of liquid from reactor mouth and first reboiler passes through pipeline connection, the first reboiler cold medium outlet and institute First rectifying column air inlet is stated by pipeline connection, the thermal medium entrance and heat source of first reboiler pass through pipeline connection, The first rectifying column tower reactor outlet is connected to the feed inlet of silicon tetrachloride storage tank by first tower reactor pump, first essence The air inlet of the gas outlet and the Second distillation column that evaporate column overhead passes through pipeline connection,
The Second distillation column tower reactor liquid outlet is connected to the refluxing opening of the first rectifying column by first reflux pump, institute The thermal medium entrance for stating Second distillation column tower top outlet and the third reboiler passes through pipeline connection, the third reboiler The entrance of thermal medium outlet and second return tank passes through pipeline connection, the outlet of second return tank and second essence The refluxing opening of tower is evaporated to be connected to by second reflux pump, the discharge port of second reflux pump also with the third distillation column Feed inlet passes through pipeline connection,
The third distillation column tower reactor outlet and the cold medium entrance of the third reboiler pass through pipeline connection, and the third is again The air inlet of the cold medium outlet and the third distillation column of boiling device passes through pipeline connection, the third distillation column tower reactor discharge port Be connected to secondary trichlorosilane reservoir inlet port by third tower reactor pump, third distillation column tower top gas outlet and described the The air inlet of three condensers passes through pipeline connection, the entrance of the condensate outlet of the third condenser and the third return tank By pipeline connection, the cold source import of the third condenser and cold source pass through pipeline connection, the outlet of the third return tank Be connected to the refluxing opening of the third distillation column by the third reflux pump, the discharge port of the third reflux pump also with purification Trichlorosilane reservoir inlet port passes through pipeline connection.
2. according to claim 1 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described First rectifying column and the Second distillation column are plate column.
3. according to claim 1 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described Third distillation column is packed tower.
4. according to any one of claims 1 to 3 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, feature exists In the first rectifying column tower top pressure is 0.28~0.35MPa, and 90~98 DEG C of the first rectifying column tower top temperature is described First rectifying column tower reactor pressure is 0.35~0.40MPa, and the first rectifying column bottom temperature is 112~117 DEG C.
5. according to claim 4 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described Second distillation column tower top pressure is 0.20~0.29MPa, 66~75 DEG C of the Second distillation column tower top temperature, second rectifying Tower tower reactor pressure is 0.27~0.34MPa, and the Second distillation column bottom temperature is 88~95 DEG C.
6. according to claim 5 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described Third distillation column tower top pressure is 0.06~0.14MPa, 44~58 DEG C of the third distillation column tower top temperature, the third rectifying Tower tower reactor pressure is 0.08~0.15MPa, 51~60 DEG C of the third distillation column bottom temperature.
7. according to claim 1 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described The heat source that first reboiler uses is that polycrystalline silicon device restores thermogenetic low-pressure steam more than process, and the low-pressure steam pressure is 0.17~0.22MPa, the low-pressure steam temperature are 130~136 DEG C.
8. according to claim 1 a kind of for restoring the Finestill energy-saving apparatus of chlorosilane purification, which is characterized in that described The cold source that third condenser uses is recirculated water, and circulating water temperature is 22~25 DEG C.
CN201822177720.1U 2018-12-24 2018-12-24 A kind of Finestill energy-saving apparatus purified for restoring chlorosilane Expired - Fee Related CN209411790U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114195098A (en) * 2022-01-06 2022-03-18 新地能源工程技术有限公司 Electronic grade hydrogen bromide preparation device and process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114195098A (en) * 2022-01-06 2022-03-18 新地能源工程技术有限公司 Electronic grade hydrogen bromide preparation device and process

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Granted publication date: 20190920