CN106744984A - The heat reclaiming system and technique of trichlorosilane production - Google Patents
The heat reclaiming system and technique of trichlorosilane production Download PDFInfo
- Publication number
- CN106744984A CN106744984A CN201611246191.5A CN201611246191A CN106744984A CN 106744984 A CN106744984 A CN 106744984A CN 201611246191 A CN201611246191 A CN 201611246191A CN 106744984 A CN106744984 A CN 106744984A
- Authority
- CN
- China
- Prior art keywords
- silicon tetrachloride
- heat
- water
- preheater
- trichlorosilane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 22
- 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 claims abstract description 61
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000007789 gas Substances 0.000 claims abstract description 42
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 42
- 239000001257 hydrogen Substances 0.000 claims abstract description 41
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000009834 vaporization Methods 0.000 claims abstract description 22
- 230000008016 vaporization Effects 0.000 claims abstract description 22
- 238000007701 flash-distillation Methods 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- 235000013312 flour Nutrition 0.000 claims description 27
- 239000000377 silicon dioxide Substances 0.000 claims description 27
- 238000005984 hydrogenation reaction Methods 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 17
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 16
- 239000005046 Chlorosilane Substances 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 10
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 4
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000004571 lime Substances 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000006200 vaporizer Substances 0.000 claims 2
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- POFAUXBEMGMSAV-UHFFFAOYSA-N [Si].[Cl] Chemical compound [Si].[Cl] POFAUXBEMGMSAV-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 125000003963 dichloro group Chemical group Cl* 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 6
- 238000005201 scrubbing Methods 0.000 description 6
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000008246 gaseous mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005373 pervaporation Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
- C01B33/10757—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane
- C01B33/10763—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material with the preferential formation of trichlorosilane from silicon
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F22—STEAM GENERATION
- F22B—METHODS OF STEAM GENERATION; STEAM BOILERS
- F22B1/00—Methods of steam generation characterised by form of heating method
- F22B1/02—Methods of steam generation characterised by form of heating method by exploitation of the heat content of hot heat carriers
- F22B1/18—Methods of steam generation characterised by form of heating method by exploitation of the heat content of hot heat carriers the heat carrier being a hot gas, e.g. waste gas such as exhaust gas of internal-combustion engines
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Combustion & Propulsion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Sustainable Energy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Silicon Compounds (AREA)
Abstract
A kind of heat reclaiming system of trichlorosilane production, including hydrogen preheater, silicon tetrachloride preheater and the silicon tetrachloride vaporization device being connected with hydrogen preheater, silicon tetrachloride preheater, the fluidized-bed reactor being also connected with electric heater including the electric heater being connected with silicon tetrachloride vaporization device and terminal condenser simultaneously.The heat reclaiming system of trichlorosilane production also includes high-temperature heat-exchanging and flash tank, high-temperature heat-exchanging is connected with flash tank and fluidized-bed reactor, water after the high-temperature heat-exchanging utilizes the cold hydrogenated tail gas heating for coming from fluidized-bed reactor to come from the water of flash tank and will heat up sends into the interior flash distillation of flash tank to produce vapor, vapor is supplied to the flash tank hydrogen preheater and silicon tetrachloride preheater as thermal source, terminal condenser is connected and the cold hydrogenated tail gas after condensing heat-exchange with high temperature water- to-water heat exchanger, to reduce production cost.The present invention also provides a kind of energy recovery technique of trichlorosilane production.
Description
Technical field
Produced the present invention relates to a kind of heat reclaiming system and technique, more particularly to a kind of trichlorosilane using cold hydrogenation
Heat reclaiming system and technique.
Background technology
Existing producing trichlorosilane by coldly hydrogenating system is using 1.2 MPas of steam to hydrogen preheater, silicon tetrachloride preheater
Exchanged heat, while material after washing is exchanged heat using recirculated cooling water, and Venturi scrubber carries out fine silicon powder
Grain removal, need to be condensed to 160 DEG C of lime set using condensed device, sprayed, washed, and cause system energy consumption higher, in system
Itself cold and hot energy utilization is not enough.Meanwhile, wash tower bottoms need to discharge silicon powder-containing granule materials, cause system loss of material,
Silica flour utilization rate is low, and needs to increase the drawbacks such as raffinate treatment process.
The content of the invention
The technical problem to be solved in the present invention is：A kind of energy recovery of the lower trichlorosilane production of production cost is provided
System, the present invention also provides a kind of energy recovery technique of the lower trichlorosilane production of production cost.
A kind of heat reclaiming system of trichlorosilane production, including hydrogen preheater, silicon tetrachloride preheater and simultaneously
The silicon tetrachloride vaporization device being connected with hydrogen preheater, silicon tetrachloride preheater, also including being connected with silicon tetrachloride vaporization device
Electric heater is connected with electric heater and carries out cold hydrogenation and produces the fluidized-bed reactor and terminal of cold hydrogenated tail gas cold
Condenser.The heat reclaiming system of trichlorosilane production also includes high-temperature heat-exchanging and flash tank, the high-temperature heat-exchanging and flash tank
It is connected with fluidized-bed reactor, the high-temperature heat-exchanging comes from sudden strain of a muscle using the cold hydrogenated tail gas heating for coming from fluidized-bed reactor
, to produce vapor, vapor is supplied to hydrogen by the flash tank to steam flash distillation in the water of groove and the water feeding flash tank after will heat up
, used as thermal source, terminal condenser is connected and the cold hydrogen after condensing heat-exchange with high temperature water- to-water heat exchanger for preheater and silicon tetrachloride preheater
Change tail gas.
A kind of energy recovery technique of trichlorosilane production, comprises the following steps:
Preheating step；Hydrogen and chlorine hydride mixed gas and silicon tetrachloride are preheated respectively using vapor；
Vaporization heating step；Hydrogen and chlorine hydride mixed gas and silicon tetrachloride are heated up using steam gasification and again together；
Cold step of hydrogenation；Hydrogen, hydrogen chloride, silicon tetrachloride and silica flour carry out cold hydrogenation in a fluidized bed reactor, produce
Cold hydrogenated tail gas；
Heat exchange flash steps；Cold hydrogenated tail gas exchange heat with desalted water and desalted water is heated up, and the desalted water flash distillation after intensification is water
Steam is used for preheating step；
Condensing steps；Cold hydrogenated tail gas condensation after by heat exchange.
The heat reclaiming system and technique of trichlorosilane production of the present invention, are produced using the heat of the tail gas after cold hydrogenation
Unboiled water steam, needs the operations such as the preheating of heat to use as thermal source supply front end, has effectively reclaimed cold hydrogenation production trichlorine
Heat during hydrogen silicon, has saved the heat consumption in production process of trichlorosilane, reduces production cost.
Brief description of the drawings
Fig. 1 is the schematic diagram of the heat reclaiming system implementation method one of trichlorosilane production of the present invention.
Fig. 2 is the schematic diagram of the heat reclaiming system implementation method two of trichlorosilane production of the present invention.
Wherein：C1 represents 0.1 MPa of steam condensate, and S2 represents 0.2 MPa of steam, and C2 represents 0.2 MPa of steam condensate,
S12 represents 1.2 MPas of steam, and C12 represents 1.2 MPas of steam condensates, and CWS represents water on recirculated water, and CWR represents that recirculated water is returned
Water.
Specific embodiment
The heat reclaiming system and technique produced to trichlorosilane of the invention with reference to diagram are described in detail.
Fig. 1 is referred to, the heat reclaiming system of the trichlorosilane production of embodiment of the present invention one includes what is be sequentially connected
Compressor air inlet surge tank 10, hydrogen preheater 11, silicon tetrachloride vaporization device 12, superheater 15, electric heater 16 and fluid bed
Reactor 17, the heat reclaiming system of trichlorosilane production also includes silicon tetrachloride storage tank 13, silicon tetrachloride preheater 14, whirlwind
Deduster 18, the first silica flour filter 19, the second silica flour filter 20, high temperature water- to-water heat exchanger 21, hot water circulating pump 22, flash tank
23rd, scrubbing tower 24, steam condensation delivery pump 25, steam condensate storage tank 26, first-stage condenser 27, terminal condenser 28, topping still
29 and chlorosilane storage tank 30.Hereinafter each equipment component will one by one be described in detail.
Compressor buffer tank 10 is connected with hydrogen preheater 11, will can be sent into after hydrogen and the boosting of a small amount of chlorination hydrogen compressed
Pre-heating temperature elevation in hydrogen preheater 11.The thermal source of hydrogen preheater 11 is 0.2 MPa of steam (S2), and hydrogen and hydrogen chloride are mixed
Gas is preheating to 120 degree.0.2 MPa of steam (S2) comes from flash tank 23, and the steam after heat exchange turns into 0.2 MPa of steam condensate
(C2) feeding steam condensate storage tank 26 is recycled.
Silicon tetrachloride storage tank 13 is connected with silicon tetrachloride preheater 14, by four chlorinations for prestoring in silicon tetrachloride storage tank 13
Preheating in silicon feeding silicon tetrachloride preheater 14.Silicon tetrachloride preheater 14 is connected with silicon tetrachloride vaporization device 12, after preheating
Hydrogen after silicon tetrachloride and preheating is sent to vaporization in silicon tetrachloride vaporization device 12 and mixes with the gaseous mixture of a small amount of hydrogen chloride.Four
The thermal source that silicon chloride preheater 11 is used is 0.2 MPa of steam (S2), silicon tetrachloride can be preheated into 130 degree, after heat exchange
Steam turn into 0.2 MPa of steam condensate (C2).Wherein, 0.2 MPa of steam (S2) comes from flash tank 23, after heat exchange
0.2 MPa of steam condensate (C2) feeding steam condensate storage tank 26 is recycled.Gaseous mixture after vaporization is proceeding through hot device 15
(600 degree) after proper temperature are heated to electric heater 16, fluidized-bed reactor 17 is sent into, entered together with the silica flour for adding
The cold hydrogenation of row, cold hydrogenated tail gas include the product trichlorosilane and dichlorosilane of cold hydrogenation, also unreacted
Complete hydrogen, hydrogen chloride, a small amount of silica flour and silicon tetrachloride.Wherein, the thermal source of superheater 15 is 1.2 MPas of steam (S12), is changed
Steam after heat turns into 1.2 MPas of steam condensate (C12), and feeding flash tank 23 is recycled.
At the top of cold hydrogenation reactor 17, cyclone dust collectors 18 are to out cold of cold hydrogenation reactor 17 for cyclone dust collectors 18
Hydrogenated tail gas carry out dedusting, remove silica flour therein.The silica flour filter 19 of cyclone dust collectors 18 and first and the second silica flour are filtered
Device 20 is connected, and tail gas is passed through into the first silica flour filter 19 and the second silica flour filter 20 carries out final dusting, further removes
Wherein remaining a small amount of fine silicon powder.
First silica flour filter 19 and the second silica flour filter 20 are parallel with one another, wherein the first silica flour filter 19 is main
Filter, the second silica flour filter 20 is reserve filter.Second silica flour filter 20 can be sent out in the first silica flour filter 19
Raw failure completes main dedusting work when blocking, maintenance system is normally run.
First silica flour filter 19 and the second silica flour filter 20 are connected after filtering silica flour with high temperature water- to-water heat exchanger 21
Cold hydrogenated tail gas contain amount of heat, about 580 degree.Cold hydrogenated tail gas are passed through high temperature water- to-water heat exchanger 21, in high temperature water- to-water heat exchanger 21
It is interior to be exchanged heat with desalted water, desalted water is heated.
High temperature water- to-water heat exchanger 21 is sequentially connected with scrubbing tower 24, first-stage condenser 27, terminal condenser 28, topping still 29,
Cold hydrogenated tail gas cooling after heat exchange in high temperature water- to-water heat exchanger 21, the chlorosilane after the washing impurity-removing of scrubbing tower 24, feeding
After first-stage condenser 27, terminal condenser 28 are condensed successively, the separating-purifying in topping still 29.Terminal condenser 28 also with compression
Machine air inlet surge tank 10 is connected, condensed a small amount of fixed gas in terminal condenser 28, including hydrogen and hydrogen chloride, is passed through pressure
Contracting machine air inlet surge tank 10 is recycled.
Topping still 29 is connected with chlorosilane storage tank 30 and silicon tetrachloride storage tank 13 simultaneously, the trichlorosilicane separated and two
Chlorine dihydro silicon feeding chlorosilane storage tank 30 is stored, used as the raw material for standby of the reduction operation of production of polysilicon.Four for separating
Silicon chloride feeding silicon tetrachloride storage tank 13 is recycled.
High temperature water- to-water heat exchanger 21 is connected with flash tank 23, hot water circulating pump 22 simultaneously, and waterway circulating is formed between three.Steam
Vapour lime set storage tank 26, steam condensate delivery pump 25 and flash tank 23 are sequentially connected, and steam condensate delivery pump 25 stores up steam condensate
The steam condensate (steam condensate falls within desalted water) of tank 26 is transported to the interior circulation of flash tank 23.
Be transported to desalted water (about 130 degree) in flash tank 23 in high temperature water- to-water heat exchanger 21 and change by hot water circulating pump 22
Heat, is heated to be 150 degree to 160 degree of high temperature desalted water, and it is 0.2 MPa ~ 0.3 MPa steaming to send back to flash distillation in flash tank 23
Vapour (S2), uses for silicon tetrachloride preheater 14, hydrogen preheater 11, topping still 29, it is also possible to access 0.2 MPa of steam pipe system
Used using steaming plant for other.0.2 MPa ~ 0.3 MPa steam is in silicon tetrachloride preheater 14, hydrogen preheater 11, thick
After evaporating the heat exchange of tower 29, steam condensate storage tank 26 is returned to as 0.1 MPa ~ 0.2 MPa steam condensate.Certainly, high temperature water- to-water heat exchanger
21 can optionally to increase be multiple.In addition, flash tank 23 can also carry out boosting design, or multiple different sizes flash tank
23, make it possible to produce simultaneously 0.2 ~ 0.3 MPa of steam (S2) supply vapor preheater 11, silicon tetrachloride preheater 14, thick
The equipment such as tower 29 are evaporated to be used using with 1.2 MPas of steam (S12) supply silicon tetrachloride vaporization devices 12 and superheater 15.
Steam condensate delivery pump 25 extracts steam condensate (C1/C2, about 0.1 to 0.2 MPa in steam condensate storage tank 26
Steam condensate) add in flash tank 23, keep flash tank 23 can continue produce steam (S2).What superheater 15 was used
After 1.2 MPas of steam (S12) turn into 1.2 MPas of steam condensates (C12) after heat exchange, it is also passed into flash tank 23 and continues to flash circulation
As 0.2 MPa ~ 0.3 MPa steam.
The energy recovery technique of the trichlorosilane production of embodiment of the present invention one comprises the following steps：
Preheating step；Hydrogen and hydrogen chloride gas and silicon tetrachloride are preheated using steam；Wherein steam is 0.2 MPa of steam
(S2) hydrogen and chlorine hydride mixed gas, are preheating to 120 degree, the preheating of hydrogen and hydrogen chloride gas is entered in hydrogen preheater 11
OK.The steam that silicon tetrachloride preheating is used is also 0.2 MPa of steam (S2), is carried out in silicon tetrachloride preheater 14, after preheating
Silicon tetrachloride temperature is 130 degree.0.2 MPa of steam (S2) of preheating comes from rear end heat exchange flash steps, pre- hot hydrogen, chlorine
Changing the steam after hydrogen and silicon tetrachloride turns into 0.2 MPa of steam condensate (C2), heat exchange flash steps is imported into again and is followed
Ring generates vapor.
Vaporization heating step；Hydrogen, hydrogen chloride and silicon tetrachloride after preheating are heated by steam again, are vaporized and rise
Temperature, temperature is further improved.Wherein, in present embodiment, pervaporation step is carried out in silicon tetrachloride vaporization device 12, is heated up in mistake
Hot device 15 is carried out, and the steam for using is 1.2 MPas of steam (S12).1.2 MPas of steam (S12) with hydrogen, hydrogen chloride and four
After silicon chloride heat exchange, as 1.2 MPas of steam condensates (C12), return to heat exchange of flash evaporation step cycle and use, after heat exchange flash distillation again
It is secondary as high-temperature high-pressure steam.The steam that the step is used is the steam that 1.2 MPas of steam (S12) can be outer confession,
Can be provided by heat exchange of flash evaporation step.Certainly, superheater 15 can also be omitted depending on circumstances.
Cold step of hydrogenation；Hydrogen, hydrogen chloride and silicon tetrachloride after vaporization intensification are heated to suitable temperature (600 degree),
Then cold hydrogenation is carried out with silica flour, trichlorosilane and dichlorosilane is generated.Wherein, hydrogen, hydrogen chloride and silicon tetrachloride
It is heated in electric heater 16, cold hydrogenation is carried out in cold hydrogenation reactor 18.Cold hydrogenation tail after cold hydrogenation
Gas, comprising trichlorosilane, the unreacted hydrogen of dichlorosilane and part, hydrogen chloride, a small amount of silica flour.
Filtration step；Cold hydrogenated tail gas remove silica flour therein by dedusting and filtering.Wherein, dedusting is anti-by cold hydrogenation
The cyclone dust collectors 18 at the top of device 17 are answered to perform, filtering is carried out by the first silica flour filter 19 and the second silica flour filter 20.
Heat exchange flash steps；Cold hydrogenated tail gas still include amount of heat (about 580 degree of temperature) after filtering, and from flash distillation
The desalted water of groove 23 is exchanged heat, and the desalted water flash distillation after heat exchange intensification is vapor, supply preheating step and/or vaporization intensification step
Suddenly use.Wherein, heat exchange is carried out in high-temperature heat-exchanging 21, and the desalted water before heat exchange is 130 degree of desalted water, de- after heat exchange
Salt solution is warmed up to about 160 degree, into flash distillation in flash tank 23 for the preheating step of 0.2 MPa of steam (S2) supply front end use with
And the separating-purifying operation of rear end is used, it is also possible to extra to flash off 1.2 MPas of part steam (S12), supply vaporization heats up and walks
Suddenly use.
Water circulation step；Preheating step turns into steam condensate after heat is lost after being exchanged heat as the vapor that thermal source is used,
Come back to heat exchange flash steps to be used as the aqueous water of heat exchange, vapor is turned into again after the flash distillation that exchanges heat, save water
Use.Similarly, the vapor that vaporization heating step is used, and the vapor that separating-purifying step (explained later) is used,
Heat exchange is equally come back to heat exchange flash steps and is used as the aqueous water of heat exchange after using.Water circulation step by pipeline and
Water pumps at different levels are carried out.
Washing step；Cold hydrogenated tail gas after heat exchange, by washing, further removal of impurities.
Condensing steps；Cold hydrogenated tail gas after washing are separated by multi-stage condensing, fixed gas therein, predominantly hydrogen and
Hydrogen chloride, feeding preheating step is recycled, and chlorosilane enters separating-purifying step.
Separating-purifying step；Chlorosilane carries out separating-purifying in topping still 29, silicon tetrachloride is separated, as original
Material feeding preheating step is recycled.Chlorosilane (including trichlorosilane and dichlorosilane) after purification is used as reduction operation
Raw material is standby to be deposited.Topping still 29 in separating-purifying step is heated using 0.2 MPa of steam (S2) for coming from heat exchange flash steps,
Steam after use turns into steam condensate and enters water circulation step, imported into heat exchange flash steps and recycles.
The heat reclaiming system and technique of trichlorosilane production of the present invention, are produced using the heat of the tail gas after cold hydrogenation
Unboiled water steam, needs the operations such as the preheating of heat to use as thermal source supply front end, has effectively reclaimed cold hydrogenation production trichlorine
Heat during hydrogen silicon, has saved the heat consumption in production process of trichlorosilane, reduces production cost.Compared to before
Production system and technique, change and reaction generation gas directly are cooled into 160 DEG C of heats not by the washing of rear system product lime set
To drawback is made full use of, while reducing first-stage condenser circulation water consumption, terminal condenser cold load is reduced.
Refer to Fig. 2, the heat reclaiming system and the class of implementation method one of the trichlorosilane production of embodiment of the present invention two
Seemingly, its difference is that a Venturi scrubber 40 is set up between high temperature water- to-water heat exchanger 21 and scrubbing tower 24, after heat exchange
Cold hydrogenated tail gas are washed in Venturi scrubber 40, further without silicon powder particle in guarantee terminal condensation liquid product, after reduction
System jams rate.Because cold hydrogenated tail gas are in the interior cooling that exchanged heat of high temperature water- to-water heat exchanger 21, so in Venturi scrubber 40
Washing can't influence overall heat recovery effect.
Correspondingly, embodiment of the present invention two trichlorosilane production energy recovery technique also with the class of implementation method one
Seemingly, difference is that washing step is divided into two steps, and Venturi scrubbing is carried out first, is carried out in Venturi scrubber 40, Ran Hou
Washed again in scrubbing tower.
In sum, presently preferred embodiments of the present invention is these are only, the scope of the present invention should not be limited with this.It is i.e. all
It is the simple equivalence changes and modification made according to claims of the present invention and description, all should still belongs to patent of the present invention
In the range of covering.
Claims (10)
1. a kind of heat reclaiming system of trichlorosilane production, including hydrogen preheater, silicon tetrachloride preheater and simultaneously with
The connected silicon tetrachloride vaporization device of hydrogen preheater, silicon tetrachloride preheater, the also electricity including being connected with silicon tetrachloride vaporization device
Heater is connected with electric heater and carries out cold hydrogenation and produces the fluidized-bed reactor and terminal of cold hydrogenated tail gas to condense
Device, it is characterised in that also including high-temperature heat-exchanging and flash tank, the high-temperature heat-exchanging and flash tank and fluidized-bed reactor phase
Even, the high-temperature heat-exchanging is come from the water of flash tank and will heat up using the cold hydrogenated tail gas heating for coming from fluidized-bed reactor
To produce vapor, vapor is supplied to hydrogen preheater and silicon tetrachloride by the flash tank for flash distillation in water feeding flash tank afterwards
Used as thermal source, terminal condenser is connected and the cold hydrogenated tail gas after condensing heat-exchange preheater with high temperature water- to-water heat exchanger.
2. the heat reclaiming system that trichlorosilane as claimed in claim 1 is produced, it is characterised in that the flash tank and four chlorinations
Silicon vaporizer is connected and provides vapor to silicon tetrachloride vaporization device as thermal source.
3. the heat reclaiming system that trichlorosilane as claimed in claim 1 is produced, it is characterised in that also including while and tetrachloro
SiClx vaporizer is connected with electric heater, will come from the superheater that the mixed gas of silicon tetrachloride vaporization device are heated, the flash distillation
Groove is connected with the superheater, and provides steam to superheater as thermal source.
4. the heat reclaiming system that trichlorosilane as claimed in claim 1 is produced, it is characterised in that also including being condensed with terminal
Device is connected, by the topping still of the chlorosilane separating-purifying of terminal condenser, the flash tank is connected with topping still and provides water vapour
To topping still as thermal source.
5. the heat reclaiming system of trichlorosilane as claimed in claim 4 production, it is characterised in that also including with topping still phase
It is used in conjunction in the silicon tetrachloride storage tank for storing the silicon tetrachloride after purifying and is connected for the chlorine silicon for storing chlorosilane with topping still
Alkane storage tank, the silicon tetrachloride storage tank is also connected with silicon tetrachloride preheater and provides silicon tetrachloride and gives silicon tetrachloride preheater.
6. the heat reclaiming system that trichlorosilane as claimed in claim 1 is produced, it is characterised in that also including for storing steaming
The steam condensate storage tank of vapour lime set and by the steam condensate in steam condensate storage tank be transported to flash tank steam condensate conveying
Pump, the steam condensate comes from the vapor after hydrogen preheater and silicon tetrachloride preheater use.
7. a kind of energy recovery technique of trichlorosilane production, comprises the following steps:
Preheating step；Hydrogen and chlorine hydride mixed gas and silicon tetrachloride are preheated respectively using vapor；
Vaporization heating step；Hydrogen and chlorine hydride mixed gas and silicon tetrachloride are heated up using steam gasification and again together；
Cold step of hydrogenation；Hydrogen, hydrogen chloride, silicon tetrachloride and silica flour carry out cold hydrogenation in a fluidized bed reactor, produce
Cold hydrogenated tail gas；
Heat exchange flash steps；Cold hydrogenated tail gas exchange heat with desalted water and desalted water is heated up, and the desalted water flash distillation after intensification is water
Steam is used for preheating step；
Condensing steps；Cold hydrogenated tail gas condensation after by heat exchange.
8. the energy recovery technique that trichlorosilane as claimed in claim 7 is produced, it is characterised in that also including filtration step；
Cold hydrogenated tail gas remove silica flour therein by dedusting and filtering.
9. the energy recovery technique that trichlorosilane as claimed in claim 7 is produced, it is characterised in that also walked including water circulation
Suddenly；The vapor used in preheating step forms steam condensate after using, and the steam condensate is directed to flash steps flash distillation and is
Water steam is utilized.
10. the energy recovery technique that trichlorosilane as claimed in claim 7 is produced, it is characterised in that also including separating-purifying
Step；The separated purification of chlorosilane after condensing steps, silicon tetrachloride feeding preheating step recycling, trichlorosilane and dichloro
Dihydro silicon is stored for future use, and the vapor that heat exchange flash steps are produced is also supplied to separating-purifying step and uses.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611246191.5A CN106744984A (en) | 2016-12-29 | 2016-12-29 | The heat reclaiming system and technique of trichlorosilane production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611246191.5A CN106744984A (en) | 2016-12-29 | 2016-12-29 | The heat reclaiming system and technique of trichlorosilane production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106744984A true CN106744984A (en) | 2017-05-31 |
Family
ID=58928908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611246191.5A Pending CN106744984A (en) | 2016-12-29 | 2016-12-29 | The heat reclaiming system and technique of trichlorosilane production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106744984A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052410A (en) * | 2018-08-27 | 2018-12-21 | 亚洲硅业（青海）有限公司 | A kind of trichlorosilane production method and its application |
| CN110980738A (en) * | 2019-12-04 | 2020-04-10 | 中国化学赛鼎宁波工程有限公司 | System and method for preparing disilane and trisilane by silane pyrolysis method |
| CN111704140A (en) * | 2020-06-29 | 2020-09-25 | 新疆协鑫新能源材料科技有限公司 | Heat energy recovery process for chlorohydrination fluidized bed |
| CN112158848A (en) * | 2020-08-24 | 2021-01-01 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN113387364A (en) * | 2021-05-08 | 2021-09-14 | 内蒙古新特硅材料有限公司 | Method and system for treating cold hydrogenation synthesis gas |
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN114477186A (en) * | 2022-01-27 | 2022-05-13 | 巴彦淖尔聚光硅业有限公司 | Cold hydrogenation production system of polycrystalline silicon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432016A (en) * | 2011-08-31 | 2012-05-02 | 上海优华系统集成技术有限公司 | Optimization recovery system for reduction tail gas heat energy in polycrystalline silicon production |
| CN104817091A (en) * | 2014-01-30 | 2015-08-05 | 内蒙古盾安光伏科技有限公司 | Treatment process of silicon tetrachloride |
-
2016
- 2016-12-29 CN CN201611246191.5A patent/CN106744984A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432016A (en) * | 2011-08-31 | 2012-05-02 | 上海优华系统集成技术有限公司 | Optimization recovery system for reduction tail gas heat energy in polycrystalline silicon production |
| CN104817091A (en) * | 2014-01-30 | 2015-08-05 | 内蒙古盾安光伏科技有限公司 | Treatment process of silicon tetrachloride |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109052410A (en) * | 2018-08-27 | 2018-12-21 | 亚洲硅业（青海）有限公司 | A kind of trichlorosilane production method and its application |
| CN109052410B (en) * | 2018-08-27 | 2020-01-10 | 亚洲硅业（青海）有限公司 | Production method and application of trichlorosilane |
| CN110980738A (en) * | 2019-12-04 | 2020-04-10 | 中国化学赛鼎宁波工程有限公司 | System and method for preparing disilane and trisilane by silane pyrolysis method |
| CN111704140A (en) * | 2020-06-29 | 2020-09-25 | 新疆协鑫新能源材料科技有限公司 | Heat energy recovery process for chlorohydrination fluidized bed |
| CN111704140B (en) * | 2020-06-29 | 2022-01-04 | 新疆协鑫新能源材料科技有限公司 | Heat energy recovery process for chlorohydrination fluidized bed |
| CN112158848A (en) * | 2020-08-24 | 2021-01-01 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| WO2022041699A1 (en) * | 2020-08-24 | 2022-03-03 | 中国恩菲工程技术有限公司 | Silicon tetrachloride cold hydrogenation system |
| CN113387364A (en) * | 2021-05-08 | 2021-09-14 | 内蒙古新特硅材料有限公司 | Method and system for treating cold hydrogenation synthesis gas |
| CN113387364B (en) * | 2021-05-08 | 2023-02-28 | 内蒙古新特硅材料有限公司 | Method and system for treating cold hydrogenation synthesis gas |
| CN114477186A (en) * | 2022-01-27 | 2022-05-13 | 巴彦淖尔聚光硅业有限公司 | Cold hydrogenation production system of polycrystalline silicon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106744984A (en) | The heat reclaiming system and technique of trichlorosilane production | |
| EP1615865B1 (en) | Apparatus and process for the production of vinyl chloride by thermal cracking of 1,2-dichloroethane | |
| CN101279735A (en) | Production method and apparatus for trichlorosilane | |
| CN102730691B (en) | Energy utilization in polysilicon hydrogenation process | |
| CN106629740A (en) | Trichlorosilane cold hydrogenation production system and process | |
| CN105084370B (en) | A kind of slurry treating method and apparatus in cold hydrogenation process | |
| CN101125276A (en) | Method for recovering tail gas of trichlorosilane production | |
| CN107418640A (en) | A kind of methanation process of effectively recovery low grade residual heat | |
| CN103449446B (en) | Method for preparing trichlorosilane | |
| CN205774201U (en) | A kind of super low energy consumption reclaims the device of caprolactam organic extractant | |
| CN107445179A (en) | The retracting device of periodic off-gases and flashed vapour in a kind of synthesis ammonia system | |
| CN107325847B (en) | Method and device for cooling and recovering waste heat of tar-containing high-temperature pyrolysis gasified gas | |
| CN110980741A (en) | Tetrachlorosilane hydrogenation system and method for preparing trichlorosilane by using same | |
| CN210861034U (en) | System for superheated water system low pressure steam | |
| CN111333484A (en) | Ultrahigh-purity methane chloride production system and process | |
| JP4914441B2 (en) | Method and apparatus for utilizing the heat of reaction generated in the production of 1,2-dichloroethane | |
| CN105565322B (en) | A kind for the treatment of method and apparatus by silicon, hydrogen and silicon tetrachloride gas/solid mixture obtained by the reaction | |
| CN217808778U (en) | Energy-saving cold hydrogenation product purification system in production of polycrystalline silicon by GCL method | |
| CN106699503B (en) | Energy-saving thermal chlorination process | |
| CN104114518B (en) | For the method and apparatus of recuperation of heat in Vinyl Chloride Monomer factory or conformability Vinyl Chloride Monomer/polrvinyl chloride factory | |
| CN211496957U (en) | Tetrachlorosilane hydrogenation system | |
| CN209411790U (en) | A kind of Finestill energy-saving apparatus purified for restoring chlorosilane | |
| CN107540508A (en) | The method and its equipment of a kind of producing phenyl ethylene by ethyl benzene catalytic dehydrogenation | |
| CN207267859U (en) | A kind of cooling of gas of high temperature pyrolysis and gasification containing tar and waste-heat recovery device | |
| CN103101942A (en) | Process for efficiently utilizing secondary steam in dissolution procedure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20201112 Address after: 015500 southeast of the intersection of jingsan road and Weisi Road, Qingshan Industrial Park, wulatehouqi, Bayannur City, Inner Mongolia Autonomous Region Applicant after: Bayannur concentrated Silicon Industry Co.,Ltd. Address before: 015543 the Inner Mongolia Autonomous Region Bayannaoer wulatehouqi Qingshan Industrial Park Applicant before: INNER MONGOLIA DUN'AN PHOTOVOLTAIC TECHNOLOGY Co.,Ltd. |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |