CN106145119B - A kind of disilane reactor - Google Patents
A kind of disilane reactor Download PDFInfo
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- CN106145119B CN106145119B CN201610469364.3A CN201610469364A CN106145119B CN 106145119 B CN106145119 B CN 106145119B CN 201610469364 A CN201610469364 A CN 201610469364A CN 106145119 B CN106145119 B CN 106145119B
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- reactor
- slag
- drip opening
- disilane
- storage tank
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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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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of disilane reactor, 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, and the storage tank is built with liquefied ammonia, the outlet discharge silane reaction mixture, the slag-drip opening discharge reaction debris, it is characterised in that the angle of the slag-drip opening and horizontal plane is 30 60 degree.Because the reactor of the present invention have selected the design of the angle of optimization design, especially slag-drip opening, deslagging speed is improved, saves the reaction time, 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 reactor.
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 reactor.
The present invention is achieved through the following technical solutions：A kind of disilane reactor, 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, and the storage tank is built with liquefied ammonia, the outlet discharge silane reaction mixing
Thing, the slag-drip opening discharge reaction debris, the angle of the slag-drip opening and horizontal plane is 30-60 degree, preferably 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.
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, improve deslagging speed, save the reaction time, production cost is relatively low,
Equipment corrosion reduces, and can be produced with continuous stabilization.
Brief description of the drawings
Fig. 1 is the structural representation of disilane reactor 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-.
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 slag-drip opening
Discharge reaction debris, the angle of the slag-drip opening and horizontal plane is 30-60 degree.
For the ease of understanding the application, now letter will be carried out using the silane product manufacturing process of the application disilane reactor
It is single 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：
NH3（l）
Mg2Si+NH4Cl----------------→SinHm+MgCl2•6NH3+H2
Catalyst
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：
MgCl2--------→Mg+Cl2
Electrolysis
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.
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 reactor, including the charging system 1 of coupled reaction kettle, storage tank 2, the outlet 3 above reactor,
The high shearing-force type blade agitators 5 of installation in the slag-drip opening 4 of reactor bottom, and reactor；The charging system is built with silicon
Change magnesium and ammonium chloride, the storage tank 2 is anti-built with liquefied ammonia, the discharge of the outlet 3 silane reaction mixture, the slag-drip opening discharge
Debris is answered, the angle of the slag-drip opening and horizontal plane is 30 degree.
Embodiment 2
Embodiment 1 is repeated, difference is, the angle of the slag-drip opening and horizontal plane is 60 degree.
Embodiment 3
Embodiment 1 is repeated, difference is, the angle of the slag-drip opening and horizontal plane is 40 degree.
Embodiment 4
Embodiment 1 is repeated, difference is, 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.
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 (3)
- A kind of 1. disilane reactor, it is characterised in that charging system, storage tank including coupled reaction kettle, above reactor The high shearing-force type blade agitators of installation in outlet, the slag-drip opening of reactor bottom, and reactor；The charging system built with Magnesium silicide and ammonium chloride, the storage tank are anti-built with liquefied ammonia, the outlet discharge silane reaction mixture, the slag-drip opening discharge Debris is answered, the angle of the slag-drip opening and horizontal plane is 40-50 degree, and the volume of the reactor is 5-10 cubic meters.
- 2. disilane reactor according to claim 1, it is characterised in that the reactor is provided with pressure detecting dress Put.
- 3. disilane reactor according to claim 1, it is characterised in that the reactor is provided with temperature detection dress Put.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610469364.3A CN106145119B (en) | 2016-06-25 | 2016-06-25 | A kind of disilane reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610469364.3A CN106145119B (en) | 2016-06-25 | 2016-06-25 | A kind of disilane reactor |
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| Publication Number | Publication Date |
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| CN106145119A CN106145119A (en) | 2016-11-23 |
| CN106145119B true CN106145119B (en) | 2018-02-27 |
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Family Cites Families (5)
| 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 |
| 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 |
| CN102936014B (en) * | 2012-10-22 | 2015-05-27 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
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2016
- 2016-06-25 CN CN201610469364.3A patent/CN106145119B/en active Active
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