CN108408734A - A kind of high-purity boron chloride preparation method and device - Google Patents
A kind of high-purity boron chloride preparation method and device Download PDFInfo
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- CN108408734A CN108408734A CN201810492240.6A CN201810492240A CN108408734A CN 108408734 A CN108408734 A CN 108408734A CN 201810492240 A CN201810492240 A CN 201810492240A CN 108408734 A CN108408734 A CN 108408734A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
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Abstract
A kind of high-purity boron chloride preparation method of present invention proposition and device, including control module, material gasification system, rectifying purification system, cold water circulating system, Mead-Bauer recovery system, exhaust treatment system, product stocking system；The material gasification system is equipped with the active and standby two sets of heating devices communicated with rectifying purification system, and the cold water circulating system is connected with rectifying purification system to maintain the condensation temperature needed for its rectifying；The rectifying purification system includes de- heavy distillation column, de-light rectification column；The tower reactor of the de- heavy distillation column is connected with Mead-Bauer recovery system to be discharged to condense the silicon tetrachloride generated as waste liquid；The offgas outlet of the de-light rectification column is with exhaust treatment system exhaust gas is discharged；The tower reactor of the de-light rectification column is connected with product stocking system to store the high-purity boron chloride product that condensation generates；The present invention can prepare the high-purity boron chloride of used in electronic industry；The purity of product is up to 99.9995%（5.5N）, total impurities content is less than 5ppm.
Description
Technical field
The present invention relates to special industrial gas generation and purification techniques field, prepared by especially a kind of high-purity boron chloride
Method and device.
Background technology
Electronic grade high-purity boron chloride is mainly used as the doped source of semiconductor silicon, is widely used in semiconductor integrated circuit
The industries such as IC, liquid crystal display LCD, light emitting semiconductor device LED and solar cell PV.In recent years, with Global Oil
Etc. energy resources gradually decrease and environmental pollution, influence of the greenhouse effects to weather, countries in the world greatly develop clean energy resource with
And power-saving technology, pay close attention to low-carbon economy.Under this background, the solar cell and light emitting semiconductor device and phase in China
Pass industry is grown rapidly, and electronic grade high-purity boron chloride market is boundless.
Invention content
A kind of high-purity boron chloride preparation method of present invention proposition and device；The high-purity tri-chlorination of used in electronic industry can be prepared
Boron；The purity of product is up to 99.9995%（5.5N）, total impurities content is less than 5ppm.
The present invention uses following technical scheme.
A kind of high-purity boron chloride preparation facilities, the preparation facilities include control module, material gasification system, rectifying
Purification system, cold water circulating system, Mead-Bauer recovery system, exhaust treatment system, product stocking system；The material gasification system
Equipped with the active and standby two sets of heating devices communicated with rectifying purification system, the heating devices heat stock bottle so that stock bottle to
Rectifying purification system exports the boron chloride steam with pressure；When the stock bottle of wherein a set of heating device exports steam pressure not
When sufficient, change from the stock bottle of another set of heating device to rectifying purification system and export steam；
The cold water circulating system is connected with rectifying purification system to maintain the condensation temperature needed for its rectifying；
The rectifying purification system includes the de- heavy distillation column being connected with material gasification system and de- heavy distillation column with boron chloride
The connected de-light rectification column of outlet conduit；The tower reactor of the de- heavy distillation column is connected that generation will be condensed with Mead-Bauer recovery system
Silicon tetrachloride as waste liquid be discharged；The offgas outlet of the de-light rectification column is with exhaust treatment system exhaust gas is discharged；It is described
The tower reactor of de-light rectification column is connected with product stocking system to store the high-purity boron chloride product that condensation generates.
The regulating valve of liquid level gauge control, the tri-chlorination in de-light rectification column tower reactor are equipped at the de-light rectification column tower reactor
When boron meets product standard, the boron chloride of de-light rectification column tower reactor is filled with product stocking system by regulating valve；When de- light rectifying
When boron chloride in tower tower reactor does not meet product standard, the boron chloride of de-light rectification column tower reactor is drained into waste liquid and returned by regulating valve
Receipts system.
It is equipped at the offgas outlet of the de-light rectification column and takes off light tail gas condenser；The Mead-Bauer recovery system and de- light tail
Gas condenser is connected with de-light rectification column tower reactor takes off light industry sequence waste liquid to collect；The Mead-Bauer recovery system is de- light industry sequence waste liquid
It is stored as the raw material of preparation facilities.
The Mead-Bauer recovery system is connected with de- heavy distillation column tower reactor takes off heavy industry sequence waste liquid to collect；When de- heavy industry sequence waste liquid
When interior content of silicon tetrachloride meets de- heavy distillation column Con trolling index, the Mead-Bauer recovery system is stored as de- heavy industry sequence waste liquid to make
The raw material of standby device.
In the tail gas of the de-light rectification column and Mead-Bauer recovery system, the boron chloride not being liquefied drains into vent gas treatment system
The hydrochloric acid trough of system generates hydrogen chloride to be reacted with water.
The de- heavy condenser boron chloride outlet conduit is equipped with sampling analysis valve；The sampling analysis valve intermittent analysis three
The content of silicon tetrachloride in boron chloride monitors the rectifying clean-up effect for taking off heavy distillation column to silicon tetrachloride, prevents silicon tetrachloride super
Mark.
The cold water circulating system and the tail gas condenser of rectifying purification system, the condenser of de-light rectification column and de- weight essence
The condenser for evaporating tower is connected；The cold water circulating system includes heat pump handpiece Water Chilling Units and press-bearing water tank；The heat pump handpiece Water Chilling Units
It prepares cold water and cold water is sent to each condenser；It is sent into after the cold water heat exchange of condenser and is recycled to press-bearing water tank from condenser, then
It is cooled down into heat pump handpiece Water Chilling Units；The water of cold water circulating system loss is automatically replenished by water compensating valve.
The preparation facilities, preparation method includes the following steps；
A1, at material gasification system electric heating cover packet in the outer wall of stock bottle, after being powered to electric heating cover, heat passes through
The outer wall of stock bottle is transmitted to boron chloride, and heating temperature and stock bottle outlet pressure are chain, and control outlet pressure is 0.6~0.8
MPa.The boron chloride steam pressure of material gasification system input rectifying purification system is controlled and is stabilized to by outlet pressure reducing valve
0.6MPa；Material gasification system takes one primary one spare steel cylinder setting, when stock bottle output pressure be less than
When 0.6MPa, which closes, and opens simultaneously spare cylinder outlet valve to maintain to supply to rectifying purification system；
Enter de- heavy distillation column after A2, the gasification of raw material boron chloride, the phegma condensed with the condenser for being taken off heavy distillation column into
Row caloic exchanges, and carries out the separation of boron chloride and silicon tetrachloride, and heavy constituent silicon tetrachloride, which is condensed, is stored in tower reactor, in de- weight essence
Under the action of evaporating tower tower reactor electric heater, the light component boron chloride in tower reactor is evaporated participates in rectifying as rising steam；It removes
When falling the boron chloride of silicon tetrachloride and being discharged from de- heavy distillation column tower top, a part is condensed and returns to de- rectifying again as phegma
Tower rectifying column, the boron chloride that another part is not condensed are discharged into de-light rectification column from condenser top；
A3, de-light rectification column carry out the separation of boron chloride and light component in raw material, in the rectifying of de-light rectification column, light component
It is discharged from overhead condenser as tail gas, the boron chloride of condensation is then stored in de-light rectification column tower reactor, is drained into as product interruption
Product storage cylinder fitted；
A4, after de-light rectification column tower reactor boron chloride impurity content reaches product standard, the tri-chlorination of de-light rectification column tower reactor
Valve enters product stocking system to boron after the adjustment；Product stocking system stores boron chloride using liquid chlorine cylinder, utilizes pressure
Difference is filled with steel cylinder from the liquid phase valve of liquid chlorine cylinder；
A5, the product stocking system take the steel cylinder of the using and the reserved to be arranged, when primary steel cylinder is full of, to weighing steel cylinder
Electronic scale will be filled with signal and be transmitted to control module, and the inlet valve of the steel cylinder is automatically closed in control system, opens simultaneously spare steel
Bottle inlet valve is to maintain the storage operation of boron chloride product.
In step A1, when needing to change stock bottle, first with the stainless steel soft of the gas valve and material gasification system of steel cylinder
Pipe connects, and replacement Treatment is carried out to stainless steel flexible hose with nitrogen, in replacement Treatment, first opens nitrogen valve and is filled with nitrogen to stock bottle
Gas to pressure rises to 0.5MPa；Nitrogen to the pressure that blow valve is released in stock bottle is opened again and is down to 0.1MPa, and repeats nitrogen
Charge and discharge operates three times.
The present invention can effectively purify boron chloride by rectifying twice, and can efficiently recycle exhaust gas, give up
Boron chloride component in liquid advantageously reduces cost, promotes economic benefit, is also beneficial to environmental protection.
Since the present invention is when raw material charges, devil liquor recovery and product dispense, it is all made of active and standby steel cylinder, therefore can make
It obtains the pressure inside the present apparatus to keep constant, helps that raw material is allowed to keep stablizing in the boiling point of rectifying, carried to ensure that this production is set
The purification quality of pure work.
Description of the drawings
The present invention is described in more detail with reference to the accompanying drawings and detailed description：
Attached drawing 1 is the schematic diagram of the material gasification system of the present invention；
Attached drawing 2 is the schematic diagram of the rectifying purification system of the present invention；
Attached drawing 3 is the schematic diagram of the cold water circulating system of the present invention；
Attached drawing 4 is the schematic diagram of the Mead-Bauer recovery system of the present invention；
Attached drawing 5 is the schematic diagram of the exhaust treatment system of the present invention；
Attached drawing 6 is the schematic diagram of product stocking system；
Attached drawing 7 is the product sub-packaging system process flow diagram being connected with product stocking system；
In figure：1- stock bottles；2- electric heating covers；3- rectifying purification systems；4- material gasification systems, 5- take off heavy distillation column；6- is de-
Light rectifying column；7- Mead-Bauer recovery systems；8- product stocking systems；9- heat pump handpiece Water Chilling Units；10- press-bearing water tanks；11- hydrochloric acid troughs.
Specific implementation mode
As shown in figs. 1-7, a kind of high-purity boron chloride preparation facilities, the preparation facilities include control module, raw material
Gasification system 4, rectifying purification system 3, cold water circulating system, Mead-Bauer recovery system 7, exhaust treatment system, product stocking system
8；The material gasification system is equipped with the active and standby two sets of heating devices communicated with rectifying purification system, the heating devices heat
Stock bottle 1 is so that stock bottle exports the boron chloride steam with pressure to rectifying purification system；When wherein a set of heating device
When stock bottle exports steam pressure deficiency, changes from the stock bottle of another set of heating device to rectifying purification system and export steam；
The cold water circulating system is connected with rectifying purification system to maintain the condensation temperature needed for its rectifying；
The rectifying purification system includes the de- heavy distillation column being connected with material gasification system and de- heavy distillation column with boron chloride
The connected de-light rectification column of outlet conduit；The tower reactor of the de- heavy distillation column is connected that generation will be condensed with Mead-Bauer recovery system
Silicon tetrachloride as waste liquid be discharged；The offgas outlet of the de-light rectification column is with exhaust treatment system exhaust gas is discharged；It is described
The tower reactor of de-light rectification column is connected with product stocking system to store the high-purity boron chloride product that condensation generates.
The regulating valve of liquid level gauge control, the tri-chlorination in de-light rectification column tower reactor are equipped at the de-light rectification column tower reactor
When boron meets product standard, the boron chloride of de-light rectification column tower reactor is filled with product stocking system by regulating valve；When de- light rectifying
When boron chloride in tower tower reactor does not meet product standard, the boron chloride of de-light rectification column tower reactor is drained into waste liquid and returned by regulating valve
Receipts system.
It is equipped at the offgas outlet of the de-light rectification column and takes off light tail gas condenser；The Mead-Bauer recovery system and de- light tail
Gas condenser is connected with de-light rectification column tower reactor takes off light industry sequence waste liquid to collect；The Mead-Bauer recovery system is de- light industry sequence waste liquid
It is stored as the raw material of preparation facilities.
The Mead-Bauer recovery system is connected with de- heavy distillation column tower reactor takes off heavy industry sequence waste liquid to collect；When de- heavy industry sequence waste liquid
When interior content of silicon tetrachloride meets de- heavy distillation column Con trolling index, the Mead-Bauer recovery system is stored as de- heavy industry sequence waste liquid to make
The raw material of standby device.
In the tail gas of the de-light rectification column and Mead-Bauer recovery system, the boron chloride not being liquefied drains into vent gas treatment system
The hydrochloric acid trough of system generates hydrogen chloride to be reacted with water.
The de- heavy condenser boron chloride outlet conduit is equipped with sampling analysis valve；The sampling analysis valve intermittent analysis three
The content of silicon tetrachloride in boron chloride monitors the rectifying clean-up effect for taking off heavy distillation column to silicon tetrachloride, prevents silicon tetrachloride super
Mark.
The cold water circulating system and the tail gas condenser of rectifying purification system, the condenser of de-light rectification column and de- weight essence
The condenser for evaporating tower is connected；The cold water circulating system includes heat pump handpiece Water Chilling Units and press-bearing water tank；The heat pump handpiece Water Chilling Units
It prepares cold water and cold water is sent to each condenser；It is sent into after the cold water heat exchange of condenser and is recycled to press-bearing water tank from condenser, then
It is cooled down into heat pump handpiece Water Chilling Units；The water of cold water circulating system loss is automatically replenished by water compensating valve.
The preparation facilities, preparation method includes the following steps；
A1, at material gasification system electric heating cover packet in the outer wall of stock bottle, after being powered to electric heating cover, heat passes through
The outer wall of stock bottle is transmitted to boron chloride, and heating temperature and stock bottle outlet pressure are chain, and control outlet pressure is 0.6~0.8
MPa.The boron chloride steam pressure of material gasification system input rectifying purification system is controlled and is stabilized to by outlet pressure reducing valve
0.6MPa；Material gasification system takes one primary one spare steel cylinder setting, when stock bottle output pressure be less than
When 0.6MPa, which closes, and opens simultaneously spare cylinder outlet valve to maintain to supply to rectifying purification system；
Enter de- heavy distillation column after A2, the gasification of raw material boron chloride, the phegma condensed with the condenser for being taken off heavy distillation column into
Row caloic exchanges, and carries out the separation of boron chloride and silicon tetrachloride, and heavy constituent silicon tetrachloride, which is condensed, is stored in tower reactor, in de- weight essence
Under the action of evaporating tower tower reactor electric heater, the light component boron chloride in tower reactor is evaporated participates in rectifying as rising steam；It removes
When falling the boron chloride of silicon tetrachloride and being discharged from de- heavy distillation column tower top, a part is condensed and returns to de- rectifying again as phegma
Tower rectifying column, the boron chloride that another part is not condensed are discharged into de-light rectification column from condenser top；
A3, de-light rectification column carry out the separation of boron chloride and light component in raw material, in the rectifying of de-light rectification column, light component
It is discharged from overhead condenser as tail gas, the boron chloride of condensation is then stored in de-light rectification column tower reactor, is drained into as product interruption
Product storage cylinder fitted；
A4, after de-light rectification column tower reactor boron chloride impurity content reaches product standard, the tri-chlorination of de-light rectification column tower reactor
Valve enters product stocking system to boron after the adjustment；Product stocking system stores boron chloride using liquid chlorine cylinder, utilizes pressure
Difference is filled with steel cylinder from the liquid phase valve of liquid chlorine cylinder；
A5, the product stocking system take the steel cylinder of the using and the reserved to be arranged, when primary steel cylinder is full of, to weighing steel cylinder
Electronic scale will be filled with signal and be transmitted to control module, and the inlet valve of the steel cylinder is automatically closed in control system, opens simultaneously spare steel
Bottle inlet valve is to maintain the storage operation of boron chloride product.
In step A1, when needing to change stock bottle, first with the stainless steel soft of the gas valve and material gasification system of steel cylinder
Pipe connects, and replacement Treatment is carried out to stainless steel flexible hose with nitrogen, in replacement Treatment, first opens nitrogen valve and is filled with nitrogen to stock bottle
Gas to pressure rises to 0.5MPa；Nitrogen to the pressure that blow valve is released in stock bottle is opened again and is down to 0.1MPa, and repeats nitrogen
Charge and discharge operates three times.
Embodiment 1：
The material gasification system process of the present invention is as shown in Figure 1, raw material boron chloride（Liquid）800 liters of steel cylinders are transported to only
Change workshop, is then connect with gasification installation.The effect of the system is to provide the trichlorine that pressure is 0.6MPa for rectifying purification system
Change boron gaseous feed, and the saturated vapour pressure of the liquid boron chloride in 800 liters of liquid chlorine cylinders at normal temperatures is 0.2MPa, therefore
Heating and gasifying must be carried out to the liquid boron chloride in 800 liters of liquid chlorine cylinders.The method that heating and gasifying uses electric heating cover, will
Electric heating cover packet is in the outer wall of 800 liters of liquid chlorine cylinders, and after being powered to electric heating cover, heat passes through the outer of 800 liters of liquid chlorine cylinders
Wall is transmitted to boron chloride, and when temperature rises to 74 DEG C, the pressure in 800 liters of liquid chlorine cylinders is 0.6MPa.Heating temperature with 800 liters
Liquid chlorine cylinder outlet pressure is chain, and control outlet pressure is 0.6~0.8 MPa.Pressure into rectifying purification system is subtracted by exporting
Pressure valve controls, it is made to stabilize to 0.6MPa.
Material gasification system takes the using and the reserved to be arranged, when 800 liters of liquid chlorine cylinder pressure are less than 0.6MPa, DCS
Outlet valve PY100a or PY100b is automatically closed in control system, opens simultaneously another 800 liters of liquid chlorine cylinder outlet valve PY100b
Or PY100a, it maintains to supply to rectifying purification system.
Since raw material steel cylinder is connect with system by stainless steel flexible hose, the raw material in steel cylinder must carry out more after being finished
It changes, when replacement must dismantle stainless steel flexible hose, because remaining boron chloride in stainless steel flexible hose, so must be with nitrogen to stainless
Steel hose carries out replacement operator.
Embodiment 2：
The rectifying purification system technological process of embodiment 2 takes off heavy distillation column as shown in Fig. 2, entering after the gasification of raw material boron chloride,
Caloic is carried out with the phegma being condensed by the condenser to exchange, and carries out the separation of boron chloride and silicon tetrachloride, four chlorination of heavy constituent
Silicon, which is condensed, is stored in tower reactor, and under the action of tower reactor electric heater, the light component boron chloride in tower reactor is evaporated as rising
Steam participates in rectifying.The boron chloride for removing silicon tetrachloride enters condenser from tower top, and a part is condensed and is returned as phegma
To rectifying column, the boron chloride that another part is not condensed is discharged into de-light rectification column from condenser top.
De-light rectification column is to carry out boron chloride and light component（Oxygen, argon, nitrogen, chlorine, carbon monoxide, carbon dioxide, methane,
Hydrogen chloride）Separation, light component is discharged from overhead condenser as tail gas, and boron chloride is then stored in tower reactor, is interrupted as product
Drain into product storage cylinder fitted.
It is equipped with sampling analysis valve AE101 in de- weight condenser boron chloride outlet conduit, four in intermittent analysis boron chloride
The content of silicon chloride monitors and takes off heavy distillation column to the rectifying clean-up effect of silicon tetrachloride, prevents silicon tetrachloride exceeded.
In de- heavy distillation column tower reactor, valve LY101 is controlled to adjust by liquid level gauge LT101, interruption is stored into four chlorinations of tower reactor
Silicon drains into Mead-Bauer recovery system as waste liquid.
It is equipped with flowmeter FT106 and regulating valve FY106 in de- condenser light offgas outlet, passes through bottom of tower sampling analysis valve
The content of light component in AE102 intermittent analysis boron chlorides makes tower reactor by the flow of regulating valve FY106 control flowmeters FT106
Boron chloride product reaches design objective.The light component being discharged from regulating valve FY106（Oxygen, argon, nitrogen, chlorine, carbon monoxide, dioxy
Change carbon, methane, hydrogen chloride）Exhaust gas recovery system is drained into as tail gas.
In de-light rectification column tower reactor, valve LY102 or LY103 are controlled to adjust by liquid level gauge LT102, when tower reactor boron chloride produces
After product qualification, boron chloride product is filled with product stocking system by regulating valve LY102.When tower reactor boron chloride product is unqualified
When, by regulating valve LY103 Mead-Bauer recovery system is drained into using boron chloride as waste liquid.
Embodiment 3：
The cold water circulating system technological process of embodiment 2 is as shown in figure 3, it is 7 DEG C that rectifying purification system condenser, which needs temperature,
Cold water makes boron chloride liquefy, and this system uses heat pump handpiece Water Chilling Units to provide cold water for condenser.The 7 of heat pump handpiece Water Chilling Units generation
DEG C cold water is sent cold water to each condenser by included water pump, and after exchanging heat with boron chloride, temperature is that 12 DEG C of cold water returns to
Press-bearing water tank, subsequently into heat pump handpiece Water Chilling Units, with this continuous cycle operation.The cold water of system loss is mended automatically by water compensating valve
Water.
Embodiment 4：
It is useless to take off heavy distillation column tower reactor as shown in figure 4, in rectifying purification process for the Mead-Bauer recovery system technological process of embodiment 3
Liquid, de-light rectification column tower reactor waste liquid, tail gas condenser waste liquid respectively enter respective Mead-Bauer recovery system.Mead-Bauer recovery system is adopted
Waste liquid is stored with 800 liters of liquid chlorine cylinders, steel cylinder is filled with from the liquid phase valve of 800 liters of liquid chlorine cylinders using pressure difference.
When it is each recycling position 800 liters of liquid chlorine cylinder pressure respectively with de- heavy distillation column tower reactor, de-light rectification column tower reactor, tail
When the pressure balance of gas condenser, waste liquid cannot enter 800 liters of liquid chlorine cylinders, therefore system be provided with row pressure regulating valve PY120,
PY130, PY140 measure 800 liters of liquid chlorine cylinder pressure, by DCS system by pressure transmitter PT120, PT130, PT140 respectively
800 liters of liquid chlorine cylinder pressure are set as 0.4MPa, when pressure superelevation, regulating valve automatically opens, and discharges 800 liters of liquid chlorine cylinder pressures
Power is to tail gas condenser.
Mead-Bauer recovery system takes the using and the reserved to be arranged, and when 800 liters of liquid chlorine cylinders are full of, electronic scale passes signal
To DCS system, DCS control systems be automatically closed inlet valve WY120a, WY130a, WY140a or WY120b, WY130b,
WY140b, open simultaneously another 800 liters of liquid chlorine cylinder inlet valves WY120b, WY130b, WY140b or WY120a, WY130a,
WY140a maintains the devil liquor recovery at each position.
The waste liquid recycled from de-light rectification column tower reactor and tail gas condenser is free of silicon tetrachloride, can be used as raw material and continues to make
With.And content of silicon tetrachloride is higher from the waste liquid that de- heavy distillation column tower reactor recycles, and is such as more than de- heavy distillation column Con trolling index, then
Raw material use is cannot function as, can send to boron chloride raw material manufacturer and handle.
Embodiment 5：
The exhaust treatment system technological process of embodiment 4 is as shown in figure 5, exhaust treatment system is mainly handled is arranged by de-light rectification column
The tail gas gone out（Oxygen, argon, nitrogen, chlorine, carbon monoxide, carbon dioxide, methane, hydrogen chloride）, wherein boron chloride content accounts for 99%, must
It must recycle, while also recycle the tail gas from Mead-Bauer recovery system.
Tail gas from de-light rectification column and Mead-Bauer recovery system enters tail gas condenser and exchanges heat with cold water, boron chloride quilt
It is condensed into liquid and drains into Mead-Bauer recovery system.The boron chloride not being liquefied drains into hydrochloric acid trough by regulating valve PY107 and is reacted with water
Hydrogen chloride is generated, the aqueous solution of hydrogen chloride is commonly called as hydrochloric acid, and 1 cubic metre of water can about dissolve 500 cubic metres of hydrogen chloride.
Embodiment 6：
The product stocking system technological process of embodiment 5 is as shown in fig. 6, when de-light rectification column tower reactor boron chloride impurity content reaches
To after product standard, valve LY102 enters product stocking system to de-light rectification column tower reactor boron chloride after the adjustment.Product stocking system
Boron chloride is stored using 930 liters of liquid chlorine cylinders, steel cylinder is filled with from the liquid phase valve of 930 liters of liquid chlorine cylinders using pressure difference.
When the pressure balance of 930 liters of product steel cylinder pressure and dehydrogenation tower bottom of rectifying tower, boron chloride cannot enter 930 liters
Product steel cylinder, therefore system is provided with row pressure regulating valve PY150, and 930 liters of product steel cylinder pressures are measured by pressure transmitter PT150
Power sets 930 liters of product steel cylinder pressure as 0.4MPa by DCS system, and when pressure superelevation, regulating valve automatically opens, discharge 930
Product steel cylinder pressure is risen to tail gas condenser.
Product stocking system takes the using and the reserved to be arranged, and when 930 liters of product steel cylinders are full of, electronic scale passes signal
To DCS system, inlet valve WY150a or WY150b is automatically closed in DCS control systems, opens simultaneously another 930 liters of product steel cylinders
Inlet valve WY150b or WY150a maintain product storage.
Embodiment 7：
The product sub-packaging system technological process of embodiment 6 is as shown in fig. 7, product sub-packaging system is by the trichlorine in 930 liters of steel cylinders
Change boron product and is dispensed into 40~50 liters of small steel cylinders.The saturated vapour pressure of liquid boron chloride at normal temperatures in 930 liters of steel cylinders is
Liquid boron chloride in 930 liters of steel cylinders is dispensed into small steel cylinder by 0.2MPa, it is necessary to the liquid trichlorine in 930 liters of steel cylinders
Change boron and carries out heating and gasifying boosting.
Heating and gasifying boosting using electric heating cover method, by electric heating cover packet in 930 liters of boron chloride product steel cylinders
Outer wall, after being powered to electric heating cover, heat is transmitted to boron chloride by the outer wall of 930 liters of product steel cylinders, when temperature rises to 74
DEG C when, the pressure in 930 liters of product steel cylinders is 0.6MPa.Heating temperature and 930 liters of steel cylinder gaseous phase outlet pressure PT160a or
PT160b is chain, and control steel cylinder is 0.6 MPa.
Boron chloride product is filled with small steel from 930 liters of product steel cylinder lower liquid phase valves through WY170a, WY170b, WY170c
Bottle, when a small steel cylinder is full of, signal is transmitted to DCS system by electronic scale, and inlet valve WY170a is automatically closed in DCS control systems
Or WY170b, WY170c, while another small steel cylinder inlet valve WY170b or WY170c are opened manually, maintain product packing.
930 liters of boron chloride product steel cylinders take the using and the reserved to be arranged, when boron chloride is fast in 930 liters of product steel cylinders
When having dispensed, 930 liters of steel cylinder gaseous phase outlet pressure PT160a or PT160b are begun to decline, and should close 930 liters of steel cylinders immediately at this time
Liquid-phase outlet valve opens another 930 liters of steel cylinder liquid-phase outlet valves, maintains product packing.
Claims (9)
1. a kind of high-purity boron chloride preparation facilities, it is characterised in that：The preparation facilities includes control module, material gasification
System, rectifying purification system, cold water circulating system, Mead-Bauer recovery system, exhaust treatment system, product stocking system；The original
Material gasification system is equipped with active and standby two sets of heating devices for being communicated with rectifying purification system, the heating devices heat stock bottle with
Stock bottle is set to export the boron chloride steam with pressure to rectifying purification system；When the stock bottle of wherein a set of heating device exports
When steam pressure deficiency, changes from the stock bottle of another set of heating device to rectifying purification system and export steam；
The cold water circulating system is connected with rectifying purification system to maintain the condensation temperature needed for its rectifying；
The rectifying purification system includes the de- heavy distillation column being connected with material gasification system and de- heavy distillation column with boron chloride
The connected de-light rectification column of outlet conduit；The tower reactor of the de- heavy distillation column is connected that generation will be condensed with Mead-Bauer recovery system
Silicon tetrachloride as waste liquid be discharged；The offgas outlet of the de-light rectification column is with exhaust treatment system exhaust gas is discharged；It is described
The tower reactor of de-light rectification column is connected with product stocking system to store the high-purity boron chloride product that condensation generates.
2. a kind of high-purity boron chloride preparation facilities according to claim 1, it is characterised in that：The de-light rectification column
It is equipped with the regulating valve of liquid level gauge control at tower reactor, when the boron chloride in de-light rectification column tower reactor meets product standard, adjusts
The boron chloride of de-light rectification column tower reactor is filled with product stocking system by valve；When the boron chloride in de-light rectification column tower reactor is not inconsistent
When closing product standard, the boron chloride of de-light rectification column tower reactor is drained into Mead-Bauer recovery system by regulating valve.
3. a kind of high-purity boron chloride preparation facilities according to claim 2, it is characterised in that：The de-light rectification column
Offgas outlet at be equipped with take off light tail gas condenser；The Mead-Bauer recovery system and de- light tail gas condenser and de-light rectification column tower
Kettle is connected takes off light industry sequence waste liquid to collect；The Mead-Bauer recovery system is stored as de- light industry sequence waste liquid the raw material of preparation facilities.
4. a kind of high-purity boron chloride preparation facilities according to claim 3, it is characterised in that：The devil liquor recovery system
System is connected with de- heavy distillation column tower reactor takes off heavy industry sequence waste liquid to collect；When content of silicon tetrachloride meets de- weight in de- heavy industry sequence waste liquid
When rectifying column Con trolling index, the Mead-Bauer recovery system is stored as de- heavy industry sequence waste liquid the raw material of preparation facilities.
5. a kind of high-purity boron chloride preparation facilities according to claim 4, it is characterised in that：The de-light rectification column
And in the tail gas of Mead-Bauer recovery system, the boron chloride not being liquefied drains into the hydrochloric acid trough of exhaust treatment system to react life with water
At hydrogen chloride.
6. a kind of high-purity boron chloride preparation facilities according to claim 1, it is characterised in that：The de- heavy condenser
Boron chloride outlet conduit is equipped with sampling analysis valve；Silicon tetrachloride contains in the sampling analysis valve intermittent analysis boron chloride
Amount monitors and takes off heavy distillation column to the rectifying clean-up effect of silicon tetrachloride, prevents silicon tetrachloride exceeded.
7. a kind of high-purity boron chloride preparation facilities according to claim 1, it is characterised in that：The circulating chilled water system
System is connected with the condenser of the tail gas condenser of rectifying purification system, the condenser of de-light rectification column and de- heavy distillation column；It is described
Cold water circulating system includes heat pump handpiece Water Chilling Units and press-bearing water tank；The heat pump handpiece Water Chilling Units prepare cold water and cold water are sent to each
Condenser；It is sent into after the cold water heat exchange of condenser and is recycled to press-bearing water tank from condenser, it is cold to enter back into the progress of heat pump handpiece Water Chilling Units
But；The water of cold water circulating system loss is automatically replenished by water compensating valve.
8. a kind of high-purity boron chloride preparation method, it is characterised in that：It is prepared by the preparation facilities in the claim 5
Method includes the following steps；
A1, at material gasification system electric heating cover packet in the outer wall of stock bottle, after being powered to electric heating cover, heat passes through
The outer wall of stock bottle is transmitted to boron chloride, and heating temperature and stock bottle outlet pressure are chain, and control outlet pressure is 0.6~0.8
Mpa；
The boron chloride steam pressure of material gasification system input rectifying purification system is controlled and is stabilized to by outlet pressure reducing valve
0.6MPa；Material gasification system takes one primary one spare steel cylinder setting, when stock bottle output pressure be less than
When 0.6MPa, which closes, and opens simultaneously spare cylinder outlet valve to maintain to supply to rectifying purification system；
Enter de- heavy distillation column after A2, the gasification of raw material boron chloride, the phegma condensed with the condenser for being taken off heavy distillation column into
Row caloic exchanges, and carries out the separation of boron chloride and silicon tetrachloride, and heavy constituent silicon tetrachloride, which is condensed, is stored in tower reactor, in de- weight essence
Under the action of evaporating tower tower reactor electric heater, the light component boron chloride in tower reactor is evaporated participates in rectifying as rising steam；It removes
When falling the boron chloride of silicon tetrachloride and being discharged from de- heavy distillation column tower top, a part is condensed and returns to de- rectifying again as phegma
Tower rectifying column, the boron chloride that another part is not condensed are discharged into de-light rectification column from condenser top；
A3, de-light rectification column carry out the separation of boron chloride and light component in raw material, in the rectifying of de-light rectification column, light component
It is discharged from overhead condenser as tail gas, the boron chloride of condensation is then stored in de-light rectification column tower reactor, is drained into as product interruption
Product storage cylinder fitted；
A4, after de-light rectification column tower reactor boron chloride impurity content reaches product standard, the tri-chlorination of de-light rectification column tower reactor
Valve enters product stocking system to boron after the adjustment；Product stocking system stores boron chloride using liquid chlorine cylinder, utilizes pressure
Difference is filled with steel cylinder from the liquid phase valve of liquid chlorine cylinder；
A5, the product stocking system take the steel cylinder of the using and the reserved to be arranged, when primary steel cylinder is full of, to weighing steel cylinder
Electronic scale will be filled with signal and be transmitted to control module, and the inlet valve of the steel cylinder is automatically closed in control system, opens simultaneously spare steel
Bottle inlet valve is to maintain the storage operation of boron chloride product.
9. a kind of high-purity boron chloride preparation method according to claim 8, it is characterised in that：In step A1, when
When needing to change stock bottle, first it is connect with the stainless steel flexible hose of material gasification system with the gas valve of steel cylinder, with nitrogen to stainless steel
Hose carries out replacement Treatment, and in replacement Treatment, first opening nitrogen valve is filled with nitrogen to pressure to stock bottle and rises to 0.5MPa；Again
It opens nitrogen to the pressure that blow valve is released in stock bottle and is down to 0.1MPa, and repeat nitrogen charge and discharge operation three times.
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| CN201810492240.6A CN108408734A (en) | 2018-05-22 | 2018-05-22 | A kind of high-purity boron chloride preparation method and device |
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| CN108821302A (en) * | 2018-09-05 | 2018-11-16 | 欧中电子材料（重庆）有限公司 | A kind of purification process and device of boron chloride |
| CN111675220A (en) * | 2020-05-08 | 2020-09-18 | 江西江氨科技有限公司 | CO is contained in tail gas generated in carbonate production2Extraction and refining system |
| CN114572992A (en) * | 2022-03-09 | 2022-06-03 | 福建福豆新材料有限公司 | Hydrogen chloride removal device for purifying boron trichloride and boron trichloride purification system |
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| US4125590A (en) * | 1977-06-29 | 1978-11-14 | Kerr-Mcgee Chemical Corporation | Method for manufacturing boron trichloride |
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| CN114572992A (en) * | 2022-03-09 | 2022-06-03 | 福建福豆新材料有限公司 | Hydrogen chloride removal device for purifying boron trichloride and boron trichloride purification system |
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