CN106115718A - A kind of Disilicoethane process units - Google Patents
A kind of Disilicoethane process units Download PDFInfo
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- CN106115718A CN106115718A CN201610469253.2A CN201610469253A CN106115718A CN 106115718 A CN106115718 A CN 106115718A CN 201610469253 A CN201610469253 A CN 201610469253A CN 106115718 A CN106115718 A CN 106115718A
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- Prior art keywords
- disilicoethane
- rectifying column
- process units
- reactor
- slag
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- 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
- C01B33/04—Hydrides of silicon
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of Disilicoethane process units, including the high shearing-force type blade agitators installed in charging system, the storage tank of coupled reaction still, the outlet above reactor, the slag-drip opening bottom reactor, and reactor；Described charging system is built with magnesium silicide and ammonium chloride, described storage tank is built with liquefied ammonia, silane reaction mixture is discharged in described outlet, the silane reaction mixture that described outlet is discharged leads to rectifying column, the tower top of described rectifying column connects condenser, and connecting at the bottom of the tower of described rectifying column has reboiler, and the Disilicoethane that described rectifying column is discharged is connected with Disilicoethane storage tank, described slag-drip opening discharges reaction foreign material, and described slag-drip opening is 30 60 degree with the angle of horizontal plane.Owing to the process units of the present invention have selected optimization design, the especially design of the angle of slag-drip opening, saving the response time, production cost is relatively low, and equipment corrosion reduces, and can produce with continuous stabilization.
Description
Technical field
The invention belongs to technical field of chemical, relate to a kind of magnesium silicide and react the dress producing Disilicoethane with ammonium chloride
Put, particularly relate to a kind of Disilicoethane process units.
Background technology
Disilicoethane is a kind of up-and-coming silicon fiml elder generation body, be in semi-conductor industry the most attractive special gas it
One.Can be used as the good raw material of amorphous si film, photochemistry fibrous raw material and siloxanes etc., at quasiconductor, photoelectric material
Have a wide range of applications in field and real value.Compared with monosilane, it has, and deposition velocity is fast, temperature requirement is low,
The superioritys such as the film uniformity is high.But, the preparation method of existing Disilicoethane mainly because productivity is low, side-product is many, relative complex, no
Being beneficial to operation causes production cost too high, which greatly limits its application.
At present, the synthetic method of Disilicoethane mainly has following several: (one), calcium-silicon enter with chlorine at 150 ~ 250 DEG C
Row gas-solid reaction [Inorganic Syntheses, 1939,1:42-45]；(2), Antaciron in the presence of ammonium chloride,
Gas-solid reaction [Journal of fluorinechemistry, 1997,83 (1), 89-is carried out with chlorine at 110 ~ 200 DEG C
91] ；(3), silicon or silicon alloy carry out chlorination and prepare Disilicoethane, wherein containing SiCl in the product obtained4、Si2Cl6, with
And Si3Cl8Above high boiling point component；Being processed by two sections of rudimentaryization, the by-product high boiling point component that i.e. (1) is initial, by adding
Heat carries out rudimentaryization reaction treatment；(2) Si of remaining3Cl8Above high boiling point component, logical chlorine carries out rudimentaryization process [day
This patent JP 59-20782]；(4), under high temperature, cracking or hydro-reduction chlorosilane carry out the pasc reaction body of deposit polycrystalline silicon
The waste gas [CN1392862A] of system's discharge；(5), chlorine and rudimentary silane (SiClX, x=0.2 ~ 0.8) and reaction so that low-grade silicon
Alkane polymerization [WO2011067331].
The Disilicoethane productivity (10 ~ 20%) the most on the low side that above method prepares, is gas-solid reaction, and device is complicated and to equipment
Requiring higher, be difficult to operation, simultaneous reactions temperature is the most higher, and energy consumption is big.These limit reaction the most to a certain extent
Promote.Therefore, development is the simplest, productivity is higher synthesis technique and equipment make it industrially obtain larger range of pushing away
Wide the most necessary, there is highly important practical significance.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of Disilicoethane process units.
The present invention is achieved through the following technical solutions: a kind of Disilicoethane process units, including the charging system of coupled reaction still
The high shearing-force type blade stirring installed in system, storage tank, the outlet above reactor, the slag-drip opening bottom reactor, and reactor
Device；Described charging system is built with magnesium silicide and ammonium chloride, and described storage tank is built with liquefied ammonia, the silane reaction that described outlet is discharged
Mixture leads to rectifying column, and the tower top of described rectifying column connects condenser, and connecting at the bottom of the tower of described rectifying column has reboiler, institute
The Disilicoethane stating rectifying column discharge delivers to Disilicoethane storage tank, and described slag-drip opening discharges reaction foreign material, described slag-drip opening and horizontal plane
Angle be 30-60 degree, preferably 40-50 degree.
Further, described reactor is provided with pressure-detecting device.
Further, described reactor is provided with temperature-detecting device.
Further, the volume of described reactor is 5-10 cubic meter.
Further, described rectifying column is the rectifying column of one group of series connection.
Further, the pipeline that described rectifying column is external is coated with heat-insulation layer.
Further, described condenser and reboiler are tubular heat exchanger.
The present invention compared with prior art has significant advantage and beneficial effect: owing to the present invention have selected optimization design
Reactor, the especially design of the angle of slag-drip opening, save the response time, production cost is relatively low, equipment corrosion reduce,
Can produce with continuous stabilization.
Accompanying drawing explanation
Fig. 1 is the structural representation of Disilicoethane process units of the present invention.
Wherein 1-charging system；2-storage tank；3-exports；4-slag-drip opening；5-height shearing-force type blade agitators；6-rectifying column；
7-condenser；8-reboiler；9-Disilicoethane storage tank.
Detailed description of the invention
For further appreciating that present disclosure, feature and effect, below in conjunction with drawings and Examples, detailed to the present invention
Explanation.
Refering to Fig. 1, a kind of Disilicoethane reactor, including charging system 1, the storage tank 2 of coupled reaction still, above reactor
The high shearing-force type blade agitators 5 installed in outlet 3, the slag-drip opening 4 bottom reactor, and reactor；In described charging system
Equipped with magnesium silicide and ammonium chloride, described storage tank 2 is built with liquefied ammonia, and silane reaction mixture, described outlet 3 are discharged in described outlet 3
The silane reaction mixture discharged leads to rectifying column 6, and the tower top of described rectifying column connects condenser 7, the tower of described rectifying column
The end connects reboiler 8, and the Disilicoethane that described rectifying column is discharged is connected with Disilicoethane storage tank 9, and it is miscellaneous that described slag-drip opening discharges reaction
Thing, described slag-drip opening is 30-60 degree with the angle of horizontal plane.
For the ease of understanding the application, the existing silane product manufacturing process by use the application Disilicoethane process units is carried out
Simple introduction.Described silane product manufacturing process comprises the steps of
A, first under 500-700 DEG C of environment, generate magnesium silicide with silica flour and magnesium powder,
Si+2Mg------→Mg2Si
B, react with ammonia chloride with magnesium silicide, in the environment of liquefied ammonia and catalyst, generate silanes and magnesium chloride hexammoniate, reaction
Formula is:
NH3(l)
Mg2Si+NH4Cl----------------→SinHm+MgCl2•6NH3+H2
Catalyst
Wherein m=2n+2
C, magnesium chloride hexammoniate are a solids product, then obtain magnesium chloride and liquefied ammonia through separating reaction in addition, and liquefied ammonia can be thrown again
Enter in above-mentioned processing procedure B and following processing procedure E and use:
MgCl2•6NH3----------→MgCl2+6NH3
D, magnesium chloride also generate magnesium powder and chlorine again through electrolysis, and magnesium powder is solid phase, can put in the A in above-mentioned processing procedure and make
With:
MgCl2--------→Mg+Cl2
Electrolysis
E, chlorine generate ammonia chloride with liquefied ammonia synthetic reaction again, and ammonia chloride is put into the B in above-mentioned processing procedure and uses, wherein liquefied ammonia
Coming from the C in above-mentioned processing procedure, in other words, the ammonia of processing procedure C generation can use for processing procedure B and E:
Cl2+H2-------→2HCl
NH3+HCl-------→NH4CL
Formula generates in step B the product of silanes from the reactions above, although monosilane and Disilicoethane are all gas, but molecule
Amount is had nothing in common with each other, and causes the temperature required difference that liquefies/gasify.Use its physical characteristic different, can respectively obtain through separating
Monosilane, Disilicoethane product, to allow the variant paraffinic product side of being individually present be answered different use demand.Specific works process
As follows: reactor admixture of gas out enters the rectification tower system of series connection, control the greenhouse cooling in rectifying tower to-1200C to-1700C, isolates Disilicoethane: cool to-170 the most again0C to-1960C, isolates monosilane.The first that will obtain
Silane is warming up to-1700More than C, makes monosilane become gas phase from liquid phase, lowers the temperature, in-1800C to-1960C temperature
In obtain high-purity monosilane；The Disilicoethane obtained is warming up to-1200More than C, makes Disilicoethane become gas phase from liquid phase, so
After lower the temperature again, in-130 0C to-1600C temperature obtains high-purity Disilicoethane, high-purity Disilicoethane is sent into Disilicoethane storage
Tank, after measured, Disilicoethane purity is up to 99.998%.
For making monosilane, Disilicoethane high precision purification, it is possible to use molecular sieve gives purification.Certainly, higher for obtaining
The purpose of precision purification, temperature difference, molecular sieve are possible not only to be used alone, and can also the two be applied in combination.Other equivalences
Purification process can be used.
Embodiment 1
Above-mentioned Disilicoethane process units, including charging system 1, the storage tank 2 of coupled reaction still, the outlet 3 above reactor, instead
The high shearing-force type blade agitators 5 installed in answering the slag-drip opening 4 in bottom portion, and reactor；Described charging system is built with silication
Magnesium and ammonium chloride, described storage tank 2 is built with liquefied ammonia, and silane reaction mixture is discharged in described outlet 3, the silicon that described outlet 3 is discharged
Alkane reactant mixture leads to rectifying column 6, and the tower top of described rectifying column connects condenser 7, and connecting at the bottom of the tower of described rectifying column has
Reboiler 8, the Disilicoethane that described rectifying column is discharged is connected with Disilicoethane storage tank 9, and described slag-drip opening discharges reaction foreign material, described row
Cinder notch is 30 degree with the angle of horizontal plane.
Embodiment 2
Repeating embodiment 1, difference is, described rectifying column is the rectifying column of 2 series connection, described slag-drip opening and horizontal plane
Angle is 60 degree.
Embodiment 3
Repeating embodiment 1, difference is, described rectifying column is the rectifying column of 3 series connection, described slag-drip opening and horizontal plane
Angle is 40 degree.
Embodiment 4
Repeating embodiment 1, difference is, described rectifying column is the rectifying column of 4 series connection, the pipeline that described rectifying column is external
Being coated with heat-insulation layer, described slag-drip opening is 50 degree with the angle of horizontal plane.
Embodiment 5
Repeat embodiment 1, further feature be the volume of reactor be 5 cubic metres.
Embodiment 6
Repeat embodiment 1, further feature be the volume of reactor be 10 cubic metres, described condenser and reboiler are row
Pipe heat exchanger.
Embodiment 7
Repeat embodiment 3, further feature be the volume of reactor be 5 cubic metres.
Embodiment 8
Repeat embodiment 4, further feature be the volume of reactor be 10 cubic metres.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member without departing from the scope of the present invention can in addition some changes, therefore the structure shown in described above comprised and accompanying drawing should
It is considered as exemplary, and is not used to limit the protection domain of patent of the present invention.
Claims (8)
1. a Disilicoethane process units, it is characterised in that include the charging system of coupled reaction still, storage tank, above reactor
Outlet, the slag-drip opening bottom reactor, and reactor in install high shearing-force type blade agitators；Described charging system is built-in
Having magnesium silicide and ammonium chloride, described storage tank is built with liquefied ammonia, and silane reaction mixture is discharged in described outlet, and described outlet is discharged
Silane reaction mixture leads to rectifying column, and the tower top of described rectifying column connects condenser, and connecting at the bottom of the tower of described rectifying column has
Reboiler, the Disilicoethane that described rectifying column is discharged delivers to Disilicoethane storage tank, described slag-drip opening discharge reaction foreign material, described slag-drip opening
It is 30-60 degree with the angle of horizontal plane.
Disilicoethane process units the most according to claim 1, it is characterised in that described slag-drip opening with the angle of horizontal plane is
40-50 degree.
Disilicoethane process units the most according to claim 1, it is characterised in that described reactor is provided with pressure detecting dress
Put.
Disilicoethane process units the most according to claim 1, it is characterised in that described reactor is provided with temperature detection dress
Put.
Disilicoethane process units the most according to claim 1, it is characterised in that the volume of described reactor is 5-10 cube
Rice.
Disilicoethane process units the most according to claim 1, it is characterised in that described rectifying column is the rectification of one group of series connection
Tower.
Disilicoethane process units the most according to claim 1, it is characterised in that the external pipeline of described rectifying column is coated with
Heat-insulation layer.
Disilicoethane process units the most according to claim 1, it is characterised in that described condenser and reboiler are tubulation
Formula heat exchanger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610469253.2A CN106115718B (en) | 2016-06-25 | 2016-06-25 | A kind of disilane process units |
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| CN201610469253.2A CN106115718B (en) | 2016-06-25 | 2016-06-25 | A kind of disilane process units |
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| CN106115718B CN106115718B (en) | 2017-11-21 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
| CN109897058A (en) * | 2019-02-28 | 2019-06-18 | 天津大学 | A kind of organic silicon slurry slag processing system and treatment process |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5526150B2 (en) * | 1975-12-29 | 1980-07-11 | ||
| JPS58156522A (en) * | 1982-03-11 | 1983-09-17 | Mitsui Toatsu Chem Inc | Preparation of disilane |
| CN102502653A (en) * | 2011-12-14 | 2012-06-20 | 浙江赛林硅业有限公司 | System and method for producing high-purity disilane |
| CN202415172U (en) * | 2011-12-19 | 2012-09-05 | 天津市泰源工业气体有限公司 | Device for producing disilane by reaction of magnesium silicide and ammonium chloride |
| CN102936014A (en) * | 2012-10-22 | 2013-02-20 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN205115061U (en) * | 2015-10-20 | 2016-03-30 | 南京亚格泰新能源材料有限公司 | Low -temperature disilane rectification device |
| CN205709892U (en) * | 2016-06-25 | 2016-11-23 | 浙江迅鼎半导体材料科技有限公司 | A kind of Disilicoethane process units |
-
2016
- 2016-06-25 CN CN201610469253.2A patent/CN106115718B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5526150B2 (en) * | 1975-12-29 | 1980-07-11 | ||
| JPS58156522A (en) * | 1982-03-11 | 1983-09-17 | Mitsui Toatsu Chem Inc | Preparation of disilane |
| CN102502653A (en) * | 2011-12-14 | 2012-06-20 | 浙江赛林硅业有限公司 | System and method for producing high-purity disilane |
| CN202415172U (en) * | 2011-12-19 | 2012-09-05 | 天津市泰源工业气体有限公司 | Device for producing disilane by reaction of magnesium silicide and ammonium chloride |
| CN102936014A (en) * | 2012-10-22 | 2013-02-20 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN205115061U (en) * | 2015-10-20 | 2016-03-30 | 南京亚格泰新能源材料有限公司 | Low -temperature disilane rectification device |
| CN205709892U (en) * | 2016-06-25 | 2016-11-23 | 浙江迅鼎半导体材料科技有限公司 | A kind of Disilicoethane process units |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950208A (en) * | 2018-06-04 | 2018-12-07 | 山东习尚喜新材料科技股份有限公司 | A kind of continuous production device and technique of metallic potassium |
| CN108950208B (en) * | 2018-06-04 | 2023-09-29 | 山东习尚喜新材料科技股份有限公司 | Continuous production device and process of metal potassium |
| CN109897058A (en) * | 2019-02-28 | 2019-06-18 | 天津大学 | A kind of organic silicon slurry slag processing system and treatment process |
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| CN106115718B (en) | 2017-11-21 |
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