CN106145119A - A kind of disilane reactor - Google Patents
A kind of disilane reactor Download PDFInfo
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- CN106145119A CN106145119A CN201610469364.3A CN201610469364A CN106145119A CN 106145119 A CN106145119 A CN 106145119A CN 201610469364 A CN201610469364 A CN 201610469364A CN 106145119 A CN106145119 A CN 106145119A
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- reactor
- drip opening
- disilane
- slag
- 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 high shearing-force type blade agitators installed in the charging system of coupled reaction kettle, storage tank, the outlet above reactor, the slag-drip opening bottom reactor, and reactor；Described charging system is built with magnesium silicide and ammonium chloride, and described storage tank is built with liquefied ammonia, and silane reaction mixture is discharged in described outlet, and described slag-drip opening discharges reaction foreign material, it is characterised in that described slag-drip opening is 30 60 degree with the angle of horizontal plane.Owing to the reactor of the present invention have selected optimization design, the especially design of the angle of slag-drip opening, improve deslagging speed, saving the reaction 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 disilane with ammonium chloride
Put, particularly relate to a kind of disilane reactor.
Background technology
Disilane is the first body of a kind of up-and-coming silicon fiml, be in semi-conductor industry quite 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 semiconductor, 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 superiority such as the film uniformity is high.But, the preparation method of existing disilane mainly because productivity is low, byproduct 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 disilane 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 is in the presence of ammonium chloride,
Carry out gas-solid reaction [Journal of fluorinechemistry, 1997,83 (1), 89-at 110 ~ 200 DEG C with chlorine
91] ；(3), silicon or silicon alloy carry out chlorination and prepare disilane, wherein contain SiCl in the product obtaining4、Si2Cl6, with
And Si3Cl8Above higher boiling component；By two sections of rudimentaryization process, i.e. (1) initial by-product higher boiling component, by adding
Heat carries out rudimentaryization reaction treatment；(2) Si of remaining3Cl8Above higher boiling 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 is polymerized [WO2011067331].
The disilane productivity (10 ~ 20%) all on the low side that above method prepares, is gas-solid reaction, and device is complicated and to equipment
Requiring higher, being difficult to operation, simultaneous reactions temperature is typically higher, and energy consumption is big.These limit reaction all to a certain extent
Promote.Therefore, develop the synthesis technique more simple, productivity is higher and equipment makes it industrially obtain larger range of pushing away
Wide very necessary, there is highly important practical significance.
Content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, a kind of disilane reactor is provided.
The present invention is achieved through the following technical solutions: a kind of disilane reactor, including the charging system of coupled reaction kettle,
The high shearing-force type blade agitators installed in storage tank, the outlet above reactor, the slag-drip opening bottom reactor, and reactor；
Described charging system is built with magnesium silicide and ammonium chloride, and described storage tank is built with liquefied ammonia, and silane reaction mixing is discharged in described outlet
Thing, described slag-drip opening discharge reaction foreign material, described slag-drip opening is 30-60 degree with the angle of horizontal plane, 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.
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, improve deslagging speed, save the reaction time, production cost is relatively low,
Equipment corrosion reduces, and can produce with continuous stabilization.
Brief description
Fig. 1 is the structural representation of disilane reactor of the present invention.
Wherein 1-charging system；2-storage tank；3-exports；4-slag-drip opening；5-height shearing-force type blade agitators.
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 disilane reactor, including the charging system of coupled reaction kettle the 1st, storage tank 2, 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 slag-drip opening are discharged in described outlet 3
Discharging reaction foreign material, 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 disilane reactor carries out letter
Single 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 sal-ammoniac 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 are obtained magnesium chloride and liquefied ammonia through separating reaction, 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 simultaneously generate magnesium powder and chlorine again through electrolysis, and magnesium powder is solid phase, and can put in the A in above-mentioned processing procedure makes
With:
MgCl2--------→Mg+Cl2
Electrolysis
E, chlorine generate sal-ammoniac with liquefied ammonia synthetic reaction again, and sal-ammoniac 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 disilane 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, disilane product, to allow the variant paraffinic product side of being individually present be answered different use demand.
For making monosilane, disilane high precision purify, it is possible to use molecular sieve is purified.Certainly, higher for obtaining
The purpose that precision purifies, 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 disilane reactor, including the charging system of coupled reaction kettle the 1st, storage tank 2, the outlet 3 above reactor, reaction
The high shearing-force type blade agitators 5 installed in the slag-drip opening 4 in bottom portion, and reactor；Described charging system is built with magnesium silicide
And ammonium chloride, described storage tank 2 is built with liquefied ammonia, and silane reaction mixture is discharged in described outlet 3, and it is miscellaneous that described slag-drip opening discharges reaction
Thing, described slag-drip opening is 30 degree with the angle of horizontal plane.
Embodiment 2
Repeating embodiment 1, difference is, described slag-drip opening is 60 degree with the angle of horizontal plane.
Embodiment 3
Repeating embodiment 1, difference is, described slag-drip opening is 40 degree with the angle of horizontal plane.
Embodiment 4
Repeating embodiment 1, difference is, 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.
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 be not used to limit the protection domain of patent of the present invention.
Claims (5)
1. a disilane reactor, it is characterised in that include charging system, the storage tank of coupled reaction kettle, above reactor
The high shearing-force type blade agitators installed in outlet, the slag-drip opening bottom reactor, and reactor；Described charging system built with
Magnesium silicide and ammonium chloride, described storage tank is built with liquefied ammonia, and silane reaction mixture is discharged in described outlet, and described slag-drip opening is discharged anti-
Answering foreign material, described slag-drip opening is 30-60 degree with the angle of horizontal plane.
2. disilane reactor according to claim 1, it is characterised in that described slag-drip opening with the angle of horizontal plane is
40-50 degree.
3. disilane reactor according to claim 1, it is characterised in that described reactor is provided with pressure detecting dress
Put.
4. disilane reactor according to claim 1, it is characterised in that described reactor is provided with temperature detection dress
Put.
5. disilane reactor according to claim 1, it is characterised in that the volume of described reactor is 5-10 cube
Rice.
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 |
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| 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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| CN106145119A true CN106145119A (en) | 2016-11-23 |
| CN106145119B CN106145119B (en) | 2018-02-27 |
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Citations (5)
| 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 |
-
2016
- 2016-06-25 CN CN201610469364.3A patent/CN106145119B/en active Active
Patent Citations (5)
| 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 |
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| CN106145119B (en) | 2018-02-27 |
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