CN110028071A - The synthesizer of trichlorosilane - Google Patents
The synthesizer of trichlorosilane Download PDFInfo
- Publication number
- CN110028071A CN110028071A CN201810029719.6A CN201810029719A CN110028071A CN 110028071 A CN110028071 A CN 110028071A CN 201810029719 A CN201810029719 A CN 201810029719A CN 110028071 A CN110028071 A CN 110028071A
- Authority
- CN
- China
- Prior art keywords
- silicon powder
- trichlorosilane
- tank
- controller
- valve group
- 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.)
- Granted
Links
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of synthesizers of trichlorosilane, comprising: silica powder drying tank, for silicon powder to be added, the pusher medium for being passed through non-oxidizing gas as silicon powder pushes silicon powder；Silicon powder charging transition tank pushes silicon powder for being passed through non-oxidizing gas as the pusher medium of silicon powder；Silicon powder surge tank, for buffering silicon powder, the pusher medium for being passed through hydrogen chloride as silicon powder pushes silicon powder；Trichlorosilane synthesis reactor, the silicon powder for being added by silicon powder surge tank generate trichlorosilane with the hcl reaction being passed through.Silicon powder surge tank in the present invention in the synthesizer of trichlorosilane, pusher medium using hydrogen chloride as silicon powder pushes silicon powder, matched nitrogen removing device in traditional trichlorosilane synthesis process can be saved, the present invention improves the partial pressure of the trichlorosilane in the synthesis gas that trichlorosilane synthetic reactor for reacting obtains, so that when being condensed during the separating-purifying of subsequent synthesis gas, trichlorosilane condensation is more complete, and the yield of trichlorosilane improves.
Description
Technical field
The invention belongs to technical field of polysilicon production, and in particular to a kind of synthesizer of trichlorosilane.
Background technique
Since two thousand five, as global new energy substitution and China's electronic industry and solar photovoltaic industry are rapidly sent out
There is explosive increase in exhibition, the polysilicon market demand, and world's photovoltaic industry is sent out at present with 31.2% annual average rate of increase high speed
Exhibition, occupies the first place of global energy GENERATION MARKET growth rate, it is contemplated that will account for world's power generation total amount to the year two thousand thirty photovoltaic power generation
30% or more, become the important energy pillar in the whole world.At present in extensive production of polysilicon, 85% factory is using improvement
Siemens Method produces polysilicon, and main raw material is trichlorosilane, thus study the production technology of trichlorosilane, production is set
Standby, production process control program, has a very important significance.
In the prior art, silicon powder and hcl reaction generate trichlorosilane in trichlorosilane synthesis reactor, usually make
It carries out pusher with nitrogen silicon powder is added in trichlorosilane synthesis reactor, but due to can not effectively prevent being introduced into for nitrogen
In trichlorosilane synthesis reactor, trichlorosilane partial pressure in synthesis gas is caused to reduce, not exclusively, product yield drops for synthesis gas condensation
It is low；Gas downstream conveying equipment row's temperature abnormality is caused to increase simultaneously, equipment runs the security risk of unstable operation.
Summary of the invention
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide a kind of trichlorine hydrogen
The synthesizer of silicon improves the partial pressure of the trichlorosilane in the synthesis gas that trichlorosilane synthetic reactor for reacting obtains, from
And when the separating-purifying of subsequent synthesis gas is condensed in the process, trichlorosilane condensation is more complete, so that trichlorine hydrogen
The yield of silicon improves.
Solve the synthesizer that technical solution used by present invention problem is to provide a kind of trichlorosilane, comprising:
Silica powder drying tank, for silicon powder to be added, when the first valve group is opened, the second valve group is closed, silica powder drying tank
The pusher medium for being also used to be passed through non-oxidizing gas as silicon powder pushes silicon powder；
Silicon powder charging transition tank, connect with silica powder drying tank, the connection between silica powder drying tank and silicon powder charging transition tank
The first valve group is provided on pipeline, when the second valve group is opened, the first valve group, third valve group are closed, silicon powder charging
Transition tank is used to be passed through non-oxidizing gas as the pusher medium of silicon powder and pushes silicon powder；
Silicon powder surge tank is connect, the connection that silicon powder feeds between transition tank and silicon powder surge tank with silicon powder charging transition tank
The second valve group is provided on pipeline, when third valve group is opened, the second valve group is closed, and silicon powder surge tank is for buffering silicon
Powder, the pusher medium for being passed through hydrogen chloride as silicon powder push silicon powder；
Trichlorosilane synthesis reactor is connect with silicon powder surge tank, silicon powder surge tank and trichlorosilane synthesis reactor it
Between connecting line on be provided with third valve group, the silicon powder that trichlorosilane synthesis reactor is used to be added by silicon powder surge tank with
The hcl reaction being passed through generates trichlorosilane.
Preferably, the synthesizer of the trichlorosilane further include:
First hydrogen chloride buffer tank is exported with silicon powder surge tank and is connected, and the first hydrogen chloride buffer tank is used for slow by silicon powder
Rush tank export be passed through into silicon powder surge tank hydrogen chloride carry out blowback.
Preferably, the synthesizer of the trichlorosilane further include:
Hydrogen chloride synthetic furnace, for providing hydrogen chloride；
First cooler is set between hydrogen chloride synthetic furnace and silicon powder surge tank, the first cooler respectively with hydrogen chloride
Synthetic furnace, the connection of silicon powder surge tank, the first cooler are used to carry out hydrogen chloride level-one cooling to obtain 140~160 DEG C of chlorination
Hydrogen is passed through 140~160 DEG C of hydrogen chloride into silicon powder surge tank and pushes silicon powder as the pusher medium of silicon powder.
Preferably, the synthesizer of the trichlorosilane further include:
Second cooler is connect with the first cooler, obtains 20~40 DEG C of chlorine for carrying out second level cooling to hydrogen chloride
Change hydrogen；
Second hydrogen chloride buffer tank is set between the second cooler and trichlorosilane synthesis reactor, the second hydrogen chloride
Surge tank is connect with the second cooler, trichlorosilane synthesis reactor respectively, and the second hydrogen chloride buffer tank is used for trichlorosilane
Raw material of 20~40 DEG C of the hydrogen chloride as synthesizing trichlorosilane is passed through in synthesis reactor.
Preferably, hydrogen chloride is room temperature hydrogen chloride.
Preferably, the outlet of the first hydrogen chloride buffer tank is connect with the entrance of the second hydrogen chloride buffer tank, the first chlorination
Hydrogen chloride in hydrogen surge tank enters pressure reduction in the second hydrogen chloride buffer tank.
Preferably, the synthesizer of the trichlorosilane further include:
First controller, the first controller connect and control with the first valve group, the second valve group, third valve group respectively
It is opened and closed.
Preferably, the synthesizer of the trichlorosilane further include:
First pressure meter, for detecting the pressure of silicon powder surge tank and being sent to the first controller；
Second pressure meter, for detecting the pressure of trichlorosilane synthesis reactor and being sent to the first controller；
First controller connect with first pressure meter, second pressure meter respectively, and the first controller is used to calculate to receive
The difference of the pressure of the pressure and trichlorosilane synthesis reactor of silicon powder surge tank, if the pressure of silicon powder surge tank subtracts trichlorine hydrogen
The difference that the pressure of silicon synthesis reactor obtains is less than preset pressure value, then the first controller control third valve group is closed.
Preferably, preset pressure value 20kPaG.
Preferably, if the first controller detects that the first valve group is opened, the first controller controls the second valve group
It closes；And/or
If the first controller detects that the second valve group is opened, the first controller controls third valve group and closes；With/
Or,
If the first controller detects that third valve group is opened, the first controller controls the second valve group and closes.
Preferably, the synthesizer of the trichlorosilane further include:
First poidometer is connect with the first controller, and the first poidometer is used to weigh the weight of the silicon powder in silica powder drying tank
The first controller is measured and is sent to, when the weight of the silicon powder in silica powder drying tank is less than preset first weight value, the first control
Device processed controls the first valve group and closes；And/or
Second poidometer is connect with the first controller, and the second poidometer is used to weigh the silicon powder in silicon powder charging transition tank
Weight and be sent to the first controller, when silicon powder charging transition tank in silicon powder weight be less than preset second weight value
When, the first controller controls the second valve group and closes；And/or
Third poidometer is connect with the first controller, and third poidometer is used to weigh the weight of the silicon powder in silicon powder surge tank
The first controller is measured and is sent to, when the weight of the silicon powder in silicon powder charging transition tank is less than preset third weight value, the
One controller controls third valve group and closes.
Preferably, the synthesizer of the trichlorosilane further include:
Refrigerant unit for cooling down to trichlorosilane synthesis reactor, the coolant quantity for adjusting refrigerant unit
Refrigerant regulating valve, temperature detecting unit, second controller, refrigerant regulating valve are connect with second controller, temperature detecting unit with
Second controller connection, temperature detecting unit is for detecting the temperature in trichlorosilane synthesis reactor and being sent to the second control
Device, if the temperature in trichlorosilane synthesis reactor reaches 355~365 DEG C, second controller control refrigerant regulating valve is opened
Degree is preset aperture, and after the preset time, second controller controls refrigerant regulating valve and closes.
Preferably, preset aperture is 30~50%, and the preset time is 20~60 seconds.
Silicon powder surge tank in the synthesizer of trichlorosilane in the present invention, the pusher using hydrogen chloride as silicon powder are situated between
Matter pushes silicon powder, can save matched nitrogen removing device in traditional trichlorosilane synthesis process, and the present invention improves trichlorosilane conjunction
At the partial pressure of the trichlorosilane in the synthesis gas reacted in reactor, so that the separating-purifying mistake of subsequent synthesis gas
When being condensed in journey, trichlorosilane condensation is more complete, so that the yield of trichlorosilane improves, reduces the fixed gas of emptying
In trichlorosilane content, thus reduce emptying waste, reduce production trichlorosilane cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the synthesizer of the trichlorosilane in the embodiment of the present invention 2.
In figure: 1- silica powder drying tank；2- silicon powder charging transition tank；3- silicon powder surge tank；4- trichlorosilane synthesis reactor；
The first valve group of 5-；The first moushroom valve of 51-；The second moushroom valve of 52-；The second valve group of 6-；61- third moushroom valve；The 4th moushroom valve of 62-；7-
Third valve group；The first hydrogen chloride buffer tank of 8-；9- hydrogen chloride synthetic furnace；The first cooler of 10-；The second cooler of 11-；12-
Second hydrogen chloride buffer tank；13- first pressure meter；14- second pressure meter；15- refrigerant unit；16- temperature detecting unit；17-
Refrigerant regulating valve.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, with reference to the accompanying drawing and specific embodiment party
Present invention is further described in detail for formula.
Embodiment 1
The present embodiment provides a kind of synthesizers of trichlorosilane, comprising:
Silica powder drying tank, for silicon powder to be added, when the first valve group is opened, the second valve group is closed, silica powder drying tank
The pusher medium for being also used to be passed through non-oxidizing gas as silicon powder pushes silicon powder；
Silicon powder charging transition tank, connect with silica powder drying tank, the connection between silica powder drying tank and silicon powder charging transition tank
The first valve group is provided on pipeline, when the second valve group is opened, the first valve group, third valve group are closed, silicon powder charging
Transition tank is used to be passed through non-oxidizing gas as the pusher medium of silicon powder and pushes silicon powder；
Silicon powder surge tank is connect, the connection that silicon powder feeds between transition tank and silicon powder surge tank with silicon powder charging transition tank
The second valve group is provided on pipeline, when third valve group is opened, the second valve group is closed, and silicon powder surge tank is for buffering silicon
Powder, the pusher medium for being passed through hydrogen chloride as silicon powder push silicon powder；
Trichlorosilane synthesis reactor is connect with silicon powder surge tank, silicon powder surge tank and trichlorosilane synthesis reactor it
Between connecting line on be provided with third valve group, the silicon powder that trichlorosilane synthesis reactor is used to be added by silicon powder surge tank with
The hcl reaction being passed through generates trichlorosilane.
Silicon powder surge tank in the synthesizer of trichlorosilane in the present embodiment, the pusher using hydrogen chloride as silicon powder
Medium pushes silicon powder, can save matched nitrogen removing device in traditional trichlorosilane synthesis process, embodiment improves trichlorine hydrogen
The partial pressure for the trichlorosilane in synthesis gas that silicon synthetic reactor for reacting obtains, so that the separation of subsequent synthesis gas mentions
When being condensed in pure procedure, trichlorosilane condensation is more complete, so that the yield of trichlorosilane improves, reduces emptying not
The content of trichlorosilane in solidifying gas reduces the cost of production trichlorosilane to reduce emptying waste.
Embodiment 2
As shown in Figure 1, the present embodiment provides a kind of synthesizers of trichlorosilane, comprising:
Silica powder drying tank 1, for silicon powder to be added, when the first valve group 5 is opened, the second valve group 6 is closed, silica powder drying
Tank 1 is also used to be passed through non-oxidizing gas as the pusher medium of silicon powder and pushes silicon powder；
Silicon powder charging transition tank 2, connect with silica powder drying tank 1, between silica powder drying tank 1 and silicon powder charging transition tank 2
The first valve group 5 is provided on connecting line, when the second valve group 6 is opened, the first valve group 5, third valve group 7 are closed,
Silicon powder charging transition tank 2 is used to be passed through non-oxidizing gas as the pusher medium of silicon powder and pushes silicon powder；
Silicon powder surge tank 3 is connect with silicon powder charging transition tank 2, and silicon powder feeds between transition tank 2 and silicon powder surge tank 3
The second valve group 6 is provided on connecting line, when third valve group 7 is opened, the second valve group 6 is closed, and silicon powder surge tank 3 is used
In buffering silicon powder, the pusher medium for being passed through hydrogen chloride as silicon powder pushes silicon powder；Specifically, the hydrogen chloride conduct in the present embodiment
Pusher medium is intermittent to be pushed into silicon powder in trichlorosilane synthesis reactor 4；
Trichlorosilane synthesis reactor 4 is connect with silicon powder surge tank 3, silicon powder surge tank 3 and trichlorosilane synthesis reactor
Third valve group 7 is provided on connecting line between 4, what trichlorosilane synthesis reactor 4 was used to be added by silicon powder surge tank 3
Silicon powder generates trichlorosilane with the hcl reaction being passed through.
The step of synthesizer of trichlorosilane in through this embodiment is fed are as follows:
The first valve group 5 is opened, the second valve group 6 is closed, non-oxidizing gas is passed through into silica powder drying tank 1, by silicon
Silicon powder in powder drying chamber 1 is sent in silicon powder charging transition tank 2；
The second valve group 6 is opened, third valve group 7 is closed, is passed through non-oxidizing gas into silicon powder charging transition tank 2,
Silicon powder in silicon powder charging transition tank 2 is sent in silicon powder surge tank 3；
Third valve group 7 is opened, the second valve group 6 is closed, is passed through hydrogen chloride into silicon powder surge tank 3, silicon powder is buffered
Silicon powder in tank 3 is sent in trichlorosilane synthesis reactor 4.
Silicon powder feeds transition tank 2 for security isolation silica powder drying tank 1 and silicon powder surge tank 3, and one side silicon powder fed
Tank 2 is crossed for preventing the nitrogen in silica powder drying tank 1 from entering in silicon powder surge tank 3, another aspect silicon powder charging transition tank 2 is used
In preventing the hydrogen chloride in silicon powder surge tank 3 from entering in silica powder drying tank 1, the safety of operator is endangered.
Preferably, non-oxidizing gas can be nitrogen, inert gas, and the non-oxidizing gas in the present embodiment is next
From the nitrogen of process engineering.
Nitrogen from process engineering is respectively used to silica powder drying tank 1, silicon powder charging transition tank 2 pushes away as pusher medium
Silicon powder intermittence is pushed into silica powder drying tank 1, silicon powder charging transition tank 2 respectively by material.
The first valve group 5 in specific the present embodiment includes: the company of the charging transition tank 2 from silica powder drying tank 1 to silicon powder
The first moushroom valve 51, the second moushroom valve 52 that adapter tube road is set gradually, the second valve group 6 include from silicon powder charging transition tank 2 to silicon
Third moushroom valve 61, the 4th moushroom valve 62 set gradually on the connecting line of powder surge tank 3, third valve group 7 include slow from silicon powder
Rush the 5th moushroom valve being arranged on tank 3 to the connecting line of trichlorosilane synthesis reactor 4.
Silicon powder surge tank 3 in the synthesizer of trichlorosilane in the present embodiment, using hydrogen chloride pushing away as silicon powder
Expect that medium pushes silicon powder, matched nitrogen removing device in traditional trichlorosilane synthesis process can be saved, embodiment improves trichlorines
The partial pressure of the trichlorosilane in synthesis gas reacted in hydrogen silicon synthesis reactor 4, so that point of subsequent synthesis gas
When from being condensed in purification process, trichlorosilane condensation is more complete, so that the yield of trichlorosilane improves, reduces emptying
Fixed gas in trichlorosilane content, thus reduce emptying waste, reduce production trichlorosilane cost.
It should be noted that the synthesizer of trichlorosilane further include:
First hydrogen chloride buffer tank 8 is exported with silicon powder surge tank 3 and is connected, and the first hydrogen chloride buffer tank 8 is for passing through silicon powder
Surge tank 3, which is exported, is passed through hydrogen chloride progress blowback into silicon powder surge tank 3.
Silicon powder suspends under the blowback effect of the hydrogen chloride from the first hydrogen chloride buffer tank 8, is effectively avoided by blowback
The blocking of the feed opening of first hydrogen chloride buffer tank 8, and the pusher of silica powder drying tank 1, silicon powder charging transition tank 2 can be prevented to be situated between
Matter non-oxidizing gas is introduced into the synthesis gas in trichlorosilane synthesis reactor 4.The silicon powder of suspension is synthesized from trichlorosilane
The upper opening of reactor 4 is added, and from the middle and lower part of trichlorosilane synthesis reactor 4, opening is passed through reaction gas hydrogen chloride, three
In chlorine hydrogen silicon synthesis reactor 4, silicon powder is under suspended state anti-with the hydrogen chloride that is passed into trichlorosilane synthesis reactor 4
Trichlorosilane and hydrogen should be generated, the silicon powder of suspended state comes into full contact with silicon powder with hydrogen chloride, is conducive to solid slope technology
It carries out.
It should be noted that the synthesizer of trichlorosilane further include:
Hydrogen chloride synthetic furnace 9, for providing hydrogen chloride；
First cooler 10, is set between hydrogen chloride synthetic furnace 9 and silicon powder surge tank 3, the first cooler 10 respectively with
Hydrogen chloride synthetic furnace 9, silicon powder surge tank 3 connect, the first cooler 10 be used to carry out hydrogen chloride level-one it is cooling obtain 140~
160 DEG C of hydrogen chloride is passed through 140~160 DEG C of hydrogen chloride into silicon powder surge tank 3 and pushes silicon as the pusher medium of silicon powder
Powder.The first cooler 10 in the present embodiment is air cooler, and 140~160 DEG C of hydrogen chloride is passed through into silicon powder surge tank 3 not only
The pusher medium push silicon powder that can be used as silicon powder, can also be dried silicon powder, prevent silicon powder from hardened, agglomeration occurs.For
The quality for ensuring above-mentioned hydrogen chloride pusher process uses the hydrogen chloride gas pair for going out dry mouth, high temperature from the first cooler 10
Silicon powder surge tank 3 carries out pressurising pusher, and silicon powder surge tank 3 maintains 0.3~0.35MPaG pressure always.
Receive the tower top of the hydrogen chloride Analytic Tower from synthesis tail gas Dry recovery process using the first hydrogen chloride buffer tank 8
Fixed gas, the main component of fixed gas are hydrogen chloride, and the pressure in the first hydrogen chloride buffer tank 8 maintains 0.5~0.55MPaG,
Simultaneously after the silicon powder blanking of silicon powder surge tank 3, the hydrogen chloride gas pair of elevated pressures in the first hydrogen chloride buffer tank 8 is used
Third valve group 7 is purged, and can to sum up be effectively prevented hydrogen chloride synthetic furnace 9 and be passed through resolving hydrochloric acid, obtained High water cut
The hardened clogging of blanking pipeline silicon powder caused by hydrogen chloride pusher is measured, the introducing of nitrogen has been prevented.
Contain chlorosilane, hydrogen chloride, hydrogen in technique of trichlorosilane synthetic tail gas.Synthesis tail gas condenses system condensing by low pressure
Afterwards, chlorosilane is condensed into liquid, and hydrogen and hydrogen chloride are still gas；The chlorosilane liquid produced being condensed is sent by pumping to chlorination
Hydrogen Analytic Tower is parsed, and wherein silicon tetrachloride and trichlorosilane are resolved out, and dichlorosilane and hydrogen chloride (carry out self-absorption
Tower) by after the tower top of Analytic Tower, then by compressor boosting, then after absorption tower is by hydrogen chloride absorption therein, obtain
Hydrogen through absorption column purification it is subsequent it is continuous send hydrogen chloride synthetic furnace 9 to use, the hydrogen chloride for being absorbed tower absorption passes through Analytic Tower parsing
After be sent to the first hydrogen chloride buffer tank 8, the second hydrogen chloride buffer tank 12.Analytic Tower is to parse the hydrogen chloride dissolved in chlorosilane
Out, the hydrogen chloride parsed is discharged in the form of fixed gas in the tower top of Analytic Tower, and 98.5% the above are chlorine in fixed gas
Change hydrogen, contains a small amount of chlorosilane.
It should be noted that the synthesizer of trichlorosilane further include:
Second cooler 11 is connect with the first cooler 10, obtains 20~40 DEG C for carrying out second level cooling to hydrogen chloride
Hydrogen chloride；
Second hydrogen chloride buffer tank 12 is set between the second cooler 11 and trichlorosilane synthesis reactor 4, the second chlorine
Change hydrogen surge tank 12 to connect with the second cooler 11, trichlorosilane synthesis reactor 4 respectively, the second hydrogen chloride buffer tank 12 is used for
Raw material of 20~40 DEG C of the hydrogen chloride as synthesizing trichlorosilane is passed through into trichlorosilane synthesis reactor 4.Synthesize trichlorine hydrogen
The reaction of silicon is exothermic reaction, and the reaction that 20~40 DEG C of hydrogen chloride is conducive to synthesizing trichlorosilane generates trichlorine hydrogen to positive reaction
The direction of silicon is mobile.In the present embodiment, the pressure in the second hydrogen chloride buffer tank 12 is 0.5~0.55MPa, and the second hydrogen chloride is slow
Tank 12 is rushed to receive from synthesis tail gas Dry recovery process Analytic Tower fixed gas.
Preferably, hydrogen chloride is room temperature hydrogen chloride.
It should be noted that the outlet of the first hydrogen chloride buffer tank 8 and the second hydrogen chloride buffer tank 12 in the present embodiment
Entrance connects, and the hydrogen chloride in the first hydrogen chloride buffer tank 8 enters pressure reduction in the second hydrogen chloride buffer tank 12.
It should be noted that the synthesizer of trichlorosilane further include:
First controller, the first controller are connect simultaneously with the first valve group 5, the second valve group 6, third valve group 7 respectively
Control its opening and closing.
Oneself of the opening and closing for the first valve group 5, the second valve group 6, third valve group 7 is realized by the first controller
Dynamic control.
It should be noted that the synthesizer of trichlorosilane further include:
First pressure meter 13, for detecting the pressure of silicon powder surge tank 3 and being sent to the first controller；
Second pressure meter 14, for detecting the pressure of trichlorosilane synthesis reactor 4 and being sent to the first controller；
First controller is connect with first pressure meter 13, second pressure meter 14 respectively, and the first controller is received for calculating
The difference of the pressure of the pressure and trichlorosilane synthesis reactor 4 of the silicon powder surge tank 3 arrived, if the pressure of silicon powder surge tank 3 subtracts
The difference for going the pressure of trichlorosilane synthesis reactor 4 to obtain is less than preset pressure value, then the first controller controls third valve
Door group 7 is closed.
Specifically, the preset pressure value in the present embodiment is 20kPaG.
It should be noted that if the first controller detects that the first valve group 5 is opened, then the first controller controls the second valve
Door group 6 is closed；The first controller detects that the first valve group 5 is opened in the present embodiment, refers to that the first controller detects the
Any one in one moushroom valve 51, the second moushroom valve 52 or two openings.
If the first controller detects that the second valve group 6 is opened, the first controller controls third valve group 7 and closes；This
The first controller detects that the second valve group 6 is opened in embodiment, refers to that the first controller detects third moushroom valve the 61, the 4th
Any one in moushroom valve 62 or two openings.
If the first controller detects that third valve group 7 is opened, the first controller controls the second valve group 6 and closes；This
The first controller detects that third valve group 7 is opened in embodiment, refers to that the first controller detects that the 5th moushroom valve is opened.
It should be noted that the synthesizer of trichlorosilane further include:
First poidometer is connect with the first controller, and the first poidometer is used to weigh the weight of the silicon powder in silica powder drying tank 1
The first controller is measured and is sent to, when the weight of the silicon powder in silica powder drying tank 1 is less than preset first weight value, the first control
Device processed controls the first valve group 5 and closes；
Second poidometer is connect with the first controller, and the second poidometer is used to weigh the silicon powder in silicon powder charging transition tank 2
Weight and be sent to the first controller, when silicon powder charging transition tank 2 in silicon powder weight be less than preset second weight value
When, the first controller controls the second valve group 6 and closes；
Third poidometer is connect with the first controller, and third poidometer is used to weigh the weight of the silicon powder in silicon powder surge tank 3
The first controller is measured and is sent to, when the weight of the silicon powder in silicon powder charging transition tank 2 is less than preset third weight value, the
One controller controls third valve group 7 and closes.
In silicon powder blanking process in silica powder drying tank 1, the first poidometer is controlled by the first controller and makes silicon powder dry
The silicon powder that 0.5~1 ton is retained in dry tank 1 can prevent silica powder drying tank 1 from mutually going here and there with the gas in silicon powder charging transition tank 2.More
It can prevent the hydrogen chloride in trichlorosilane synthesis reactor 4 from escaping by silica powder drying tank 1, avoid hydrogen chloride to operator
Injury.
In the silicon powder blanking process that silicon powder feeds in transition tank 2, the second poidometer is controlled by the first controller and makes silicon
The silicon powder that 0.5~1 ton is retained in powder charging transition tank 2, can prevent the gas in silicon powder charging transition tank 2 and silicon powder surge tank 3
Body is mutually gone here and there.
In silicon powder blanking process in silicon powder surge tank 3, third poidometer is controlled by the first controller and makes silicon powder slow
It rushes in tank 3 and retains 0.5~1 ton of silicon powder, silicon powder surge tank 3 and the gas in trichlorosilane synthesis reactor 4 can be prevented mutual
String.
Specifically, preset first weight value is 0.5~1 ton in the present embodiment, preset second weight value is 0.5~1
Ton, preset third weight value are 0.5~1 ton.
It should be noted that the synthesizer of trichlorosilane further include:
Refrigerant unit 15 for cooling down to trichlorosilane synthesis reactor 4, for adjusting the cold of refrigerant unit 15
The refrigerant regulating valve 17 of medium flow, temperature detecting unit 16, second controller, refrigerant regulating valve 17 and second controller connect
It connects, temperature detecting unit 16 is connect with second controller, and temperature detecting unit 16 is for detecting in trichlorosilane synthesis reactor 4
Temperature and be sent to second controller, if temperature in trichlorosilane synthesis reactor 4 reaches 355~365 DEG C, the second control
The aperture of device control refrigerant regulating valve 17 processed is preset aperture, and after the preset time, second controller controls refrigerant tune
Valve 17 is saved to close.By second controller by the temperature stability contorting in trichlorosilane synthesis reactor 4 at 355~365 DEG C, prevent
When only reaction temperature is lower than 280 DEG C, reactivity sharply declines, and dichloro-dihydro silicone content increases in synthesis gas, or even reaction meeting
It can not start；When reaction temperature can also be prevented to be greater than 355~365 DEG C, side reaction, which occurs, leads to the silicon tetrachloride in synthesis gas
Content increases, and product yield reduces.Specifically, the temperature detecting unit 16 in the present embodiment is thermocouple.
Preferably, the preset aperture of refrigerant regulating valve 17 is 30~50%, and the preset time is 20~60 seconds.Specifically
, the preset aperture of the refrigerant regulating valve 17 in the present embodiment is 40%, and the preset time is 45 seconds.
In the prior art, influence 4 temperature of trichlorosilane synthesis reactor because being known as: the density of silicon powder particle, partial size, stream
The multiple factors such as mass flowrate, fluid density, the fluid viscosity of body.Simultaneously according to from the point of view of practical production experience with the cycle of operation
Rising, can also have individual difference in the temperature control of every trichlorosilane synthesis reactor 4.The superposition of above-mentioned factor so that
The control of 4 temperature of trichlorosilane synthesis reactor realizes that automatic control is abnormal difficult, even if the Advanced Control Techniques that come into operation also do not provide
Good solution realizes the automatic control of the temperature of trichlorosilane synthesis reactor 4.
The application is freed from prison disk operation by second controller, by the operator for producing trichlorosilane, is kept away
The a large amount of energy of operator of consumption trichlorosilane is exempted from.However production practical experience is combined to pass through the control in second controller
Increase refrigerant in system and adjust timing control logic, can effectively evade influences the temperature controlled of trichlorosilane synthesis reactor 4
Factors, can be realized the automatic control of trichlorosilane synthesis reactor 4, effectively ensure trichlorosilane synthesis reactor 4
The steady and product yield of interior reaction mitigates labor intensity of operating staff, reduces the manpower of trichlorosilane synthesis process production
Cost.The present embodiment realizes the automatic control of trichlorosilane synthesis manpower temperature of reactor, effectively ensures that trichlorosilane boils
The steady and product yield of bed reaction effectively reduces trichlorosilane synthesis process production human cost.
The synthesis gas that trichlorosilane synthesis reactor 4 in the present embodiment comes out, it is laggard by cyclonic separation, bag-type dust
Enter wet sprinkling dust-removing process, then condensed through chlorosilane cooler, obtains liquid phase crude product and be sent to the purification removal of impurities of raw material workshop, obtain
To gas phase tail gas send to the isolated high-purity hydrogen of synthesis tail gas Dry recovery process and be sent into hydrogen chloride synthetic furnace 9, with chlorine
It is reacted in hydrogen chloride synthetic furnace 9, recycles it further, the hydrogen chloride of production is used as synthesis after being condensed, being dried
The raw material of trichlorosilane, is sent into trichlorosilane synthesis reactor 4, and such synthesis tail gas just all returns to trichlorosilane and synthesizes work
Sequence completes material closed cycle.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (9)
1. a kind of synthesizer of trichlorosilane characterized by comprising
Silica powder drying tank, for silicon powder to be added, when the first valve group is opened, the second valve group is closed, and silica powder drying tank is also used
Silicon powder is pushed in being passed through pusher medium of the non-oxidizing gas as silicon powder；
Silicon powder charging transition tank, connect with silica powder drying tank, the connecting line between silica powder drying tank and silicon powder charging transition tank
On be provided with the first valve group, when the second valve group open when, the first valve group, third valve group close, silicon powder feed transition
Tank is used to be passed through non-oxidizing gas as the pusher medium of silicon powder and pushes silicon powder；
Silicon powder surge tank is connect, the connecting line that silicon powder feeds between transition tank and silicon powder surge tank with silicon powder charging transition tank
On be provided with the second valve group, when third valve group is opened, the second valve group is closed, silicon powder surge tank for buffering silicon powder,
The pusher medium that hydrogen chloride is passed through as silicon powder pushes silicon powder；
Trichlorosilane synthesis reactor is connect with silicon powder surge tank, between silicon powder surge tank and trichlorosilane synthesis reactor
Be provided with third valve group on connecting line, the silicon powder that trichlorosilane synthesis reactor is used to be added by silicon powder surge tank be passed through
Hcl reaction generate trichlorosilane.
2. the synthesizer of trichlorosilane according to claim 1, which is characterized in that further include:
First hydrogen chloride buffer tank is exported with silicon powder surge tank and is connected, and the first hydrogen chloride buffer tank is used to pass through silicon powder surge tank
It exports and is passed through hydrogen chloride progress blowback into silicon powder surge tank.
3. the synthesizer of trichlorosilane according to claim 1, which is characterized in that further include:
Hydrogen chloride synthetic furnace, for providing hydrogen chloride；
First cooler is set between hydrogen chloride synthetic furnace and silicon powder surge tank, the first cooler respectively with hydrogen chloride synthesis
Furnace, the connection of silicon powder surge tank, the first cooler are used to carry out hydrogen chloride level-one cooling to obtain 140~160 DEG C of hydrogen chloride, to
It is passed through 140~160 DEG C of hydrogen chloride in silicon powder surge tank and pushes silicon powder as the pusher medium of silicon powder.
4. the synthesizer of trichlorosilane according to claim 3, which is characterized in that further include:
Second cooler is connect with the first cooler, obtains 20~40 DEG C of hydrogen chloride for carrying out second level cooling to hydrogen chloride；
Second hydrogen chloride buffer tank is set between the second cooler and trichlorosilane synthesis reactor, the second hydrogen chloride buffering
Tank is connect with the second cooler, trichlorosilane synthesis reactor respectively, and the second hydrogen chloride buffer tank is used to synthesize to trichlorosilane
Raw material of 20~40 DEG C of the hydrogen chloride as synthesizing trichlorosilane is passed through in reactor.
5. the synthesizer of trichlorosilane according to claim 1, which is characterized in that further include:
First controller, the first controller connect with the first valve group, the second valve group, third valve group respectively and control it and open
It closes.
6. the synthesizer of trichlorosilane according to claim 5, which is characterized in that further include:
First pressure meter, for detecting the pressure of silicon powder surge tank and being sent to the first controller；
Second pressure meter, for detecting the pressure of trichlorosilane synthesis reactor and being sent to the first controller；
First controller is connect with first pressure meter, second pressure meter respectively, and the first controller is for calculating the silicon powder received
The difference of the pressure of the pressure and trichlorosilane synthesis reactor of surge tank, if the pressure of silicon powder surge tank subtracts trichlorosilane conjunction
It is less than preset pressure value at the difference that the pressure of reactor obtains, then the first controller control third valve group is closed.
7. the synthesizer of trichlorosilane according to claim 5, which is characterized in that if the first controller detects first
Valve group is opened, then the first controller controls the second valve group and closes；And/or
If the first controller detects that the second valve group is opened, the first controller controls third valve group and closes；And/or
If the first controller detects that third valve group is opened, the first controller controls the second valve group and closes.
8. the synthesizer of trichlorosilane according to claim 5, which is characterized in that further include:
First poidometer is connect with the first controller, and the first poidometer is used to weigh the weight of the silicon powder in silica powder drying tank simultaneously
It is sent to the first controller, when the weight of the silicon powder in silica powder drying tank is less than preset first weight value, the first controller
Control the closing of the first valve group；And/or
Second poidometer is connect with the first controller, and the second poidometer is used to weigh the weight of the silicon powder in silicon powder charging transition tank
The first controller is measured and is sent to, when the weight of the silicon powder in silicon powder charging transition tank is less than preset second weight value, the
One controller controls the second valve group and closes；And/or
Third poidometer is connect with the first controller, and third poidometer is used to weigh the weight of the silicon powder in silicon powder surge tank simultaneously
It is sent to the first controller, when the weight of the silicon powder in silicon powder charging transition tank is less than preset third weight value, the first control
Device control third valve group processed is closed.
9. the synthesizer of trichlorosilane according to claim 1, which is characterized in that further include:
The refrigerant of refrigerant unit for cooling down to trichlorosilane synthesis reactor, the coolant quantity for adjusting refrigerant unit
Regulating valve, temperature detecting unit, second controller, refrigerant regulating valve are connect with second controller, temperature detecting unit and second
Controller connection, temperature detecting unit are used to detect the temperature in trichlorosilane synthesis reactor and are sent to second controller,
If the temperature in trichlorosilane synthesis reactor reaches 355~365 DEG C, the aperture of second controller control refrigerant regulating valve is
Preset aperture, after the preset time, second controller controls refrigerant regulating valve and closes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810029719.6A CN110028071B (en) | 2018-01-12 | 2018-01-12 | Trichlorosilane synthesis device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810029719.6A CN110028071B (en) | 2018-01-12 | 2018-01-12 | Trichlorosilane synthesis device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110028071A true CN110028071A (en) | 2019-07-19 |
| CN110028071B CN110028071B (en) | 2021-01-22 |
Family
ID=67234441
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810029719.6A Active CN110028071B (en) | 2018-01-12 | 2018-01-12 | Trichlorosilane synthesis device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110028071B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254387A (en) * | 2007-12-04 | 2008-09-03 | 魏玺群 | Voltage transformation adsorption method for separating mixture gas containing hydrogen and chloro-silicane and/or hydrogenchloride mixture gas |
| CN101279735A (en) * | 2008-05-30 | 2008-10-08 | 中蓝晨光化工研究院有限公司 | Production method and apparatus for trichlorosilane |
| CN102040223A (en) * | 2010-12-23 | 2011-05-04 | 江西嘉柏新材料有限公司 | Method for producing trichlorosilane by continuously adding silicon powder |
| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN203440098U (en) * | 2013-07-08 | 2014-02-19 | 昆明冶研新材料股份有限公司 | Silica powder conveying equipment and trichlorosilane synthesizing system with same |
-
2018
- 2018-01-12 CN CN201810029719.6A patent/CN110028071B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254387A (en) * | 2007-12-04 | 2008-09-03 | 魏玺群 | Voltage transformation adsorption method for separating mixture gas containing hydrogen and chloro-silicane and/or hydrogenchloride mixture gas |
| CN101279735A (en) * | 2008-05-30 | 2008-10-08 | 中蓝晨光化工研究院有限公司 | Production method and apparatus for trichlorosilane |
| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN102040223A (en) * | 2010-12-23 | 2011-05-04 | 江西嘉柏新材料有限公司 | Method for producing trichlorosilane by continuously adding silicon powder |
| CN203440098U (en) * | 2013-07-08 | 2014-02-19 | 昆明冶研新材料股份有限公司 | Silica powder conveying equipment and trichlorosilane synthesizing system with same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110028071B (en) | 2021-01-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108793169A (en) | A kind of square law device and system recycling Buddha's warrior attendant wire cutting silicon material by-product silicon mud | |
| CN101279735A (en) | Production method and apparatus for trichlorosilane | |
| CN107445138B (en) | polycrystalline silicon reduction tail gas recovery method and recovery system | |
| CN103043616A (en) | Device and method for preparing high-purity oxygen gas based on chemical-loop air separation technique | |
| CN106139890B (en) | The device and method of cold-rolled steel sheet heat treatment nitrogen hydrogen mixed tail gas recycling purification | |
| CN101239723A (en) | Plasma producing method and device for polycrystalline silicon | |
| CN102502646B (en) | Equipment and method for preparing polysilicon by fast circulating fluidized bed-based chemical vapor deposition | |
| CN104628038B (en) | A kind of flaorination process reclaiming fluorine gas | |
| CN110963494B (en) | System and method for preparing silane | |
| CN107540020B (en) | A kind of synthetic method of tungsten hexafluoride | |
| CN102515099A (en) | Membrane separation method and device for recycling hydrogen from purge gas of synthetic ammonia liquid ammonia storage tank | |
| CN110028071A (en) | The synthesizer of trichlorosilane | |
| CN101759187B (en) | Preparation method and device for solar-grade polycrystalline silicon | |
| CN106698438B (en) | Coupled polycrystalline silicon production system | |
| WO2024027341A1 (en) | Method for cleaning deposited silicon on inner wall of fluidized bed | |
| CN102815702B (en) | Device and process of producing high-purity granular polycrystalline silicon by silanizing fluidized bed | |
| CN203529947U (en) | Silicon powder recovery device for producing silicon tetrachloride by adopting direct method | |
| CN109734104B (en) | Device and method for producing ammonia water by using purge gas system of synthetic ammonia | |
| CN104891499A (en) | Technological method for preparing polysilicon by silane method | |
| CN217699212U (en) | Preparation device of high-purity nitric oxide | |
| CN201850148U (en) | Silicon powder drying device | |
| CN109317693A (en) | A method of germanium metal is directly prepared using germanium tetrachloride | |
| CN205099363U (en) | System for production silicon nitride | |
| CN102786092B (en) | Vertical countercurrent fluorinated furnace used for producing tungsten hexafluoride and use method thereof | |
| CN111268682B (en) | Composition for preparing polycrystalline silicon, preparation method and preparation system |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20190719 Assignee: Inner Mongolia Xinte silicon material Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000326 Denomination of invention: Synthesis device of trichlorosilane Granted publication date: 20210122 License type: Common License Record date: 20220627 Application publication date: 20190719 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2022990000325 Denomination of invention: Synthesis device of trichlorosilane Granted publication date: 20210122 License type: Common License Record date: 20220627 |
|
| EE01 | Entry into force of recordation of patent licensing contract |