CN106115718B - A kind of disilane process units - Google Patents
A kind of disilane process units Download PDFInfo
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- CN106115718B CN106115718B CN201610469253.2A CN201610469253A CN106115718B CN 106115718 B CN106115718 B CN 106115718B CN 201610469253 A CN201610469253 A CN 201610469253A CN 106115718 B CN106115718 B CN 106115718B
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- disilane
- rectifying column
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- slag
- process units
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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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Abstract
The invention discloses a kind of disilane process units, including the charging system of coupled reaction kettle, storage tank, the outlet above reactor, the high shearing-force type blade agitators of installation in the slag-drip opening of reactor bottom, and reactor；The charging system is built with magnesium silicide and ammonium chloride, the storage tank is built with liquefied ammonia, the outlet discharge silane reaction mixture, the silane reaction mixture of the outlet discharge leads to rectifying column, the tower top of the rectifying column is connected with condenser, and the bottom of towe of the rectifying column is connected with reboiler, and the disilane of the rectifying column discharge is connected with disilane storage tank, the slag-drip opening discharge reaction debris, the angle of the slag-drip opening and horizontal plane is 30 60 degree.Because the process units of the present invention have selected the design of the angle of optimization design, especially slag-drip opening, the reaction time is saved, production cost is relatively low, and equipment corrosion reduces, and can be produced with continuous stabilization.
Description
Technical field
The invention belongs to technical field of chemical, is related to the dress that a kind of magnesium silicide produces disilane with ammonium chloride reaction
Put, more particularly to a kind of disilane process units.
Background technology
Disilane is a kind of up-and-coming silicon fiml elder generation body, be in semi-conductor industry quite attractive special gas it
One.It can be used as the good raw material of amorphous si film, photochemistry fibrous raw material and siloxanes etc., in semiconductor, photoelectric material
Had a wide range of applications Deng field and real value.Compared with monosilane, it has, and deposition velocity is fast, temperature requirement is low,
The superiority such as film uniformity height.But the preparation method of existing disilane is mainly because low yield, byproduct are more, relative complex, no
Cause production cost too high beneficial to operation, which greatly limits its application.
At present, the synthetic method of disilane mainly has following several：（One）, calcium-silicon enters at 150 ~ 250 DEG C with chlorine
Row gas-solid reaction [Inorganic Syntheses, 1939,1:42-45] ；（Two）, Antaciron in the presence of ammonium chloride,
Gas-solid reaction [Journal of fluorinechemistry, 1997,83 (1), 89- are carried out in 110 ~ 200 DEG C and chlorine
91] ；（Three）, silicon or silicon alloy carry out chlorination and prepare disilane, wherein containing SiCl in obtained product4、Si2Cl6, with
And Si3Cl8Higher boiling component above；Handled by two sections of rudimentaryization, i.e.,（1）Initial by-product higher boiling component, by adding
Heat carries out rudimentaryization reaction treatment；（2）The Si of remaining3Cl8Higher boiling component above, lead to chlorine and carry out rudimentaryization processing [day
This patent JP 59-20782]；（Four）, cracking or hydro-reduction chlorosilane carry out the pasc reaction body of deposit polycrystalline silicon under high temperature
It is the waste gas [CN1392862A] of discharge；（Five）, chlorine and rudimentary silane（SiClX, x=0.2 ~ 0.8）Reaction so that low-grade silicon
Alkane polymerize [WO2011067331].
Disilane yield is all relatively low made from above method（10~20%）, it is gas-solid reaction, device is complicated and to equipment
It is required that higher, not easy to operate, simultaneous reactions temperature is typically higher, and energy consumption is big.These all limit reaction to a certain extent
Promote.Therefore, developing the synthesis technique more simple, yield is higher and equipment makes it industrially obtain larger range of push away
It is wide very necessary, there is highly important practical significance.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of disilane process units.
The present invention is achieved through the following technical solutions：A kind of disilane process units, include the charging system of coupled reaction kettle
Unite, storage tank, the outlet above reactor, the slag-drip opening of reactor bottom, and the high shearing-force type blade stirring of the interior installation of reactor
Device；The charging system is built with magnesium silicide and ammonium chloride, and the storage tank is built with liquefied ammonia, the silane reaction of the outlet discharge
Mixture leads to rectifying column, and the tower top of the rectifying column is connected with condenser, and the bottom of towe of the rectifying column is connected with reboiler, institute
The disilane for stating rectifying column discharge is sent to disilane storage tank, the slag-drip opening discharge reaction debris, the slag-drip opening and horizontal plane
Angle be 30-60 degree, preferred 40-50 degree.
Further, the reactor is provided with pressure-detecting device.
Further, the reactor is provided with temperature-detecting device.
Further, the volume of the reactor is 5-10 cubic meters.
Further, the rectifying column is the rectifying column of one group of series connection.
Further, the external pipeline of the rectifying column is coated with heat-insulation layer.
Further, the condenser and reboiler are tubular heat exchanger.
The present invention has the advantages of notable and beneficial effect compared with prior art：Because the present invention have selected optimization design
Reactor, the especially angle of slag-drip opening design, save the reaction time, production cost is relatively low, equipment corrosion reduce,
It can be produced with continuous stabilization.
Brief description of the drawings
Fig. 1 is the structural representation of disilane process units of the present invention.
Wherein 1- charging systems；2- storage tanks；3- is exported；4- slag-drip openings；The high shearing-force type blade agitators of 5-；6- rectifying columns；
7- condensers；8- reboilers；9- disilane storage tanks.
Embodiment
It is detailed to the present invention below in conjunction with drawings and Examples to further appreciate that present disclosure, feature and effect
Explanation.
Refering to Fig. 1, a kind of disilane reactor, including the charging system 1 of coupled reaction kettle, storage tank 2, above reactor
The high shearing-force type blade agitators 5 of installation in outlet 3, the slag-drip opening 4 of reactor bottom, and reactor；In the charging system
Equipped with magnesium silicide and ammonium chloride, the storage tank 2 is built with liquefied ammonia, the discharge of the outlet 3 silane reaction mixture, the outlet 3
The silane reaction mixture of discharge leads to rectifying column 6, and the tower top of the rectifying column is connected with condenser 7, the tower of the rectifying column
Bottom is connected with reboiler 8, and the disilane of the rectifying column discharge is connected with disilane storage tank 9, and the slag-drip opening discharge reaction is miscellaneous
Thing, the angle of the slag-drip opening and horizontal plane is 30-60 degree.
For the ease of understanding the application, will now be carried out using the silane product manufacturing process of the application disilane process units
It is simple to introduce.The silane product manufacturing process comprises the steps of：
A, magnesium silicide is generated under 500-700 DEG C of environment with silica flour and magnesium powder first,
Si+2Mg------→Mg2Si
B, reacted with magnesium silicide and sal-ammoniac, in the environment of liquefied ammonia and catalyst, generate silanes and magnesium chloride hexammoniate,
Reaction equation is：
Wherein m=2n+2
C, magnesium chloride hexammoniate is a solids product, then obtains magnesium chloride and liquefied ammonia through being separated reaction, and liquefied ammonia can be with
Put into above-mentioned processing procedure B and following processing procedure E and use again：
MgCl2•6NH3----------→MgCl2+6NH3
D, magnesium chloride and magnesium powder and chlorine are generated through electrolysis again, magnesium powder is solid phase, can be put into the A in above-mentioned processing procedure
Use：
E, chlorine generates sal-ammoniac with liquefied ammonia synthetic reaction again, and the B that sal-ammoniac is able to put into above-mentioned processing procedure is used, wherein
Liquefied ammonia comes from the C in above-mentioned processing procedure, and in other words, the ammonia of processing procedure C generations can use for processing procedure B and E：
Cl2+H2-------→2HCl
NH3+HCl-------→NH4CL
Generate the product of silanes in formula in step B from the reactions above, although monosilane and disilane are all gas,
Molecular weight is had nothing in common with each other, and causes temperature needed for liquefaction/gasification different.It is different with its physical characteristic, it can distinguish by separation
Monosilane, disilane product are obtained, to allow the variant paraffinic product side of being individually present to be able to answer different use demands.Specific works
Process is as follows：Reactor come out admixture of gas enter series connection rectifying column group, control rectifying tower in greenhouse cooling to-
120 0C to -1700C, isolate disilane：Then -170 are cooled to again0C to -1960C, isolate monosilane.It will obtain
Monosilane be warming up to -1700More than C, monosilane is become gas phase from liquid phase, then cool again, in -1800C to -1960C
High-purity monosilane is obtained in temperature；Obtained disilane is warming up to -1200More than C, disilane is set to become gas from liquid phase
Phase, then cool again, in -130 0C to -1600High-purity disilane is obtained in C temperature, high-purity disilane is sent into second silicon
Alkane storage tank, after measured, disilane purity is up to 99.998%.
To make monosilane, the purifying of disilane high precision, can be purified using molecular sieve.Certainly, it is higher to obtain
The purpose of precision purifying, temperature difference, molecular sieve not only can be used alone, can also the two be applied in combination.Other it is equivalent it
Purification process can be used.
Embodiment 1
Above-mentioned disilane process units, including the charging system 1 of coupled reaction kettle, storage tank 2, the outlet above reactor
3, the slag-drip opening 4 of reactor bottom, and the high shearing-force type blade agitators 5 of the interior installation of reactor；The charging system built with
Magnesium silicide and ammonium chloride, the storage tank 2 is built with liquefied ammonia, the discharge of the outlet 3 silane reaction mixture, the discharge of outlet 3
Silane reaction mixture lead to rectifying column 6, the tower top of the rectifying column is connected with condenser 7, and the bottom of towe of the rectifying column connects
Reboiler 8 is connected to, the disilane of the rectifying column discharge is connected with disilane storage tank 9, the slag-drip opening discharge reaction debris, institute
The angle for stating slag-drip opening and horizontal plane is 30 degree.
Embodiment 2
Embodiment 1 is repeated, difference is, the rectifying column is the rectifying column of 2 series connection, the slag-drip opening and level
The angle in face is 60 degree.
Embodiment 3
Embodiment 1 is repeated, difference is, the rectifying column is the rectifying column of 3 series connection, the slag-drip opening and level
The angle in face is 40 degree.
Embodiment 4
Embodiment 1 is repeated, difference is, the rectifying column is the rectifying column of 4 series connection, and the rectifying column is external
Pipeline is coated with heat-insulation layer, and the angle of the slag-drip opening and horizontal plane is 50 degree.
Embodiment 5
Embodiment 1 is repeated, further feature is that the volume of reactor is 5 cubic metres.
Embodiment 6
Embodiment 1 is repeated, further feature is that the volume of reactor is 10 cubic metres, and the condenser and reboiler are equal
For tubular heat exchanger.
Embodiment 7
Embodiment 3 is repeated, further feature is that the volume of reactor is 5 cubic metres.
Embodiment 8
Embodiment 4 is repeated, further feature is that the volume of reactor is 10 cubic metres.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member can be subject to some changes not departing from the scope of the present invention, therefore the structure shown in described above included and accompanying drawing should
It is considered as protection domain that is exemplary, and being not used to limit patent of the present invention.
Claims (7)
1. a kind of disilane process units, it is characterised in that charging system, storage tank including coupled reaction kettle, reactor top
Outlet, the slag-drip opening of reactor bottom, and reactor in installation high shearing-force type blade agitators；The charging system is built-in
There are magnesium silicide and ammonium chloride, the storage tank is built with liquefied ammonia, and silane reaction mixture is discharged in the outlet, the outlet discharge
Silane reaction mixture leads to rectifying column, and the tower top of the rectifying column is connected with condenser, and the bottom of towe of the rectifying column is connected with
Reboiler, the condenser and reboiler are tubular heat exchanger, and the disilane of the rectifying column discharge is sent to disilane storage
Tank, the slag-drip opening discharge reaction debris, the angle of the slag-drip opening and horizontal plane is 30-60 degree.
2. disilane process units according to claim 1, it is characterised in that the angle of the slag-drip opening and horizontal plane is
40-50 degree.
3. disilane process units according to claim 1, it is characterised in that the reactor is provided with pressure detecting dress
Put.
4. disilane process units according to claim 1, it is characterised in that the reactor is provided with temperature detection dress
Put.
5. disilane process units according to claim 1, it is characterised in that the volume of the reactor is 5-10 cubes
Rice.
6. disilane process units according to claim 1, it is characterised in that the rectifying column is the rectifying of one group of series connection
Tower.
7. disilane process units according to claim 1, it is characterised in that the external pipeline of the rectifying column is coated with
Heat-insulation layer.
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| Application Number | Priority Date | Filing Date | Title |
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| 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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| CN106115718A CN106115718A (en) | 2016-11-16 |
| CN106115718B true CN106115718B (en) | 2017-11-21 |
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| 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 |
Citations (5)
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|---|---|---|---|---|
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5283419A (en) * | 1975-12-29 | 1977-07-12 | Shin Etsu Chem Co Ltd | Preparation of methylchlorosilanes |
| JPS58156522A (en) * | 1982-03-11 | 1983-09-17 | Mitsui Toatsu Chem Inc | Preparation of disilane |
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2016
- 2016-06-25 CN CN201610469253.2A patent/CN106115718B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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