CN113083166A - Disilane preparation equipment and preparation method - Google Patents
Disilane preparation equipment and preparation method Download PDFInfo
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- CN113083166A CN113083166A CN202110280743.9A CN202110280743A CN113083166A CN 113083166 A CN113083166 A CN 113083166A CN 202110280743 A CN202110280743 A CN 202110280743A CN 113083166 A CN113083166 A CN 113083166A
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- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 107
- 238000010438 heat treatment Methods 0.000 claims abstract description 71
- 238000000926 separation method Methods 0.000 claims abstract description 60
- 230000003197 catalytic effect Effects 0.000 claims abstract description 40
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 22
- 238000007599 discharging Methods 0.000 claims abstract description 8
- 239000002912 waste gas Substances 0.000 claims abstract description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 107
- 238000001816 cooling Methods 0.000 claims description 56
- 239000012495 reaction gas Substances 0.000 claims description 46
- 239000012263 liquid product Substances 0.000 claims description 40
- 229910000077 silane Inorganic materials 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 20
- 239000012535 impurity Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910021487 silica fume Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 230000009467 reduction Effects 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 238000005979 thermal decomposition reaction Methods 0.000 description 5
- -1 lithium aluminum hydride Chemical compound 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000005686 electrostatic field Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000012280 lithium aluminium hydride Substances 0.000 description 2
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 2
- 229910021338 magnesium silicide Inorganic materials 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910007264 Si2H6 Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides disilane preparation equipment and a disilane preparation method. The disilane preparation equipment comprises a heating device, a first gas inlet, a second gas outlet, a gas inlet and a gas outlet, wherein the heating device is provided with the first gas inlet and the first gas outlet; a catalytic dehydrogenation reactor having a second gas inlet and a second gas outlet; the cryogenic device is provided with a third air inlet, a third liquid outlet and a third waste gas outlet; the light component removing and separating tower is provided with a fourth feeding hole, a fourth gas outlet and a fourth liquid outlet; the adsorption device is provided with a fifth feeding hole and a fifth discharging hole; and the de-heavy separation tower is provided with a sixth feeding hole, a sixth gas outlet and a sixth liquid outlet. Therefore, the disilane preparation equipment provided by the embodiment of the invention has the advantages of high disilane conversion rate, high production efficiency, reduction of resource waste, reduction of production cost and the like.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to disilane preparation equipment and a disilane preparation method.
Background
Disilane (Si2H6) is an advanced film-forming electronic specialty gas, and has the characteristics of lower deposition temperature, faster film-forming rate, higher film uniformity and the like in a film deposition process compared with other silicon source gases, and many advanced integrated circuit chip manufacturers have come into wide use at present. In the related art, there are three main techniques for producing disilane, namely (1) synthesis of magnesium silicide and ammonium chloride. The method takes magnesium silicide and ammonia chloride as raw materials, generates silane in the presence of liquid ammonia and a catalyst, and simultaneously produces disilane gas as a byproduct, so that disilane is less in proportion and low in production efficiency. (2) A halodisilane reduction method. The reaction uses lithium aluminum hydride or sodium aluminum hydride to reduce hexachlorodisilane to prepare disilane, and the complexing metal hydride such as lithium aluminum hydride or sodium aluminum hydride is used to reduce hexachlorodisilane to prepare disilane. The adopted raw material hexachlorodisilane is expensive, is not easy to obtain, has low purity, and has slow reaction speed in a solvent and low production efficiency. And in the reaction process, an organic silicon compound can be produced as a byproduct, so that the separation is difficult, and impurities are easily introduced in the process, so that the product quality is influenced. (3) The direct silane synthesizing process has silane as initial material and through atom excitation, thermal decomposition, photolysis, electrostatic field, glow discharge and other steps, silane may be converted into disilane. However, the method has low conversion rate, brown yellow amorphous silicon solid substances are easily generated in the process, and the industrial application value is not high.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. To this end, the embodiment of the invention provides disilane preparation equipment.
The disilane preparation equipment according to the embodiment of the invention comprises:
a heating device having a first air inlet and a first air outlet;
the catalytic dehydrogenation reactor is provided with a second gas inlet and a second gas outlet, and the second gas inlet is communicated with the first gas outlet;
the cryogenic device is provided with a third air inlet, a third liquid outlet and a third waste gas outlet, and the third air inlet is communicated with the second air outlet;
the light component removing and separating tower is provided with a fourth feeding hole, a fourth gas outlet and a fourth liquid outlet, the fourth feeding hole is communicated with the third liquid outlet, and the fourth gas outlet is communicated with the first gas inlet;
the adsorption device is provided with a fifth feeding hole and a fifth discharging hole, and the fifth feeding hole is communicated with the fourth liquid outlet; and
and the de-weight separation tower is provided with a sixth feeding hole, a sixth gas outlet and a sixth liquid outlet, and the sixth feeding hole is communicated with the fifth discharging hole.
Therefore, the disilane preparation equipment provided by the embodiment of the invention has the advantages of high disilane conversion rate, high production efficiency, reduction of resource waste, reduction of production cost and the like.
In some embodiments, the compressor further comprises a seventh gas inlet and a seventh gas outlet, the seventh gas inlet is connected to the second gas outlet, and the seventh gas outlet is communicated with the third gas inlet.
In some embodiments, further comprising:
a first precision filter having a first filter inlet and a first filter outlet, the first filter inlet being connected to the first gas outlet, the first filter outlet being connected to the second gas inlet; and
and the second precision filter is provided with a second filtering inlet and a second filtering outlet, the second filtering inlet is connected with the second air outlet, and the second filtering outlet is connected with the seventh air inlet.
In some embodiments, further comprising:
the first preheater comprises a first heating cavity and a first cooling cavity, the first heating cavity is matched with the first cooling cavity, the first heating cavity is provided with a first heating inlet and a first heating outlet, the first cooling cavity is provided with a first cooling inlet and a first cooling outlet, the first heating outlet is connected with the first air inlet, the first cooling inlet is connected with the second filtering outlet, and the first cooling outlet is connected with the seventh air inlet; and
the second preheater comprises a second heating cavity and a second cooling cavity, the second heating cavity is matched with the second cooling cavity, the second heating cavity is provided with a second heating inlet and a second heating outlet, the second cooling cavity is provided with a second cooling inlet and a second cooling outlet, the second cooling inlet is connected with the seventh gas outlet, the second cooling outlet is connected with the third gas inlet, the second heating inlet is connected with the fourth gas outlet, and the second heating outlet is connected with the first heating inlet.
In some embodiments, the catalytic dehydrogenation reactor is a tubular reactor, and the catalytic dehydrogenation reactor is loaded with a catalyst, optionally the catalyst comprises at least one of oxides of zinc, nickel, iron, and copper.
In some embodiments, a porous support is disposed within the catalytic dehydrogenation reactor, optionally the porous support comprises activated carbon, alumina, and a molecular sieve.
The application also provides a disilane preparation method implemented by the disilane preparation equipment, which comprises the following steps:
A) heating monosilane by using the heating device so as to heat the temperature of the monosilane to 100-250 ℃;
B) introducing the heated monosilane into the catalytic dehydrogenation reactor to perform catalytic dehydrogenation reaction so as to obtain mixed reaction gas, wherein the mixed reaction gas comprises disilane, hydrogen, higher-order silane and monosilane, and the catalytic dehydrogenation reaction is performed at the temperature of 100-250 ℃ and under the condition of 0.2MPaG-0.4 MpaG;
C) cooling the mixed reaction gas by using the cryogenic device so as to obtain non-condensable gas and liquid products, wherein the liquid products comprise one part of the monosilane, the disilane and the high-order silane, the non-condensable gas comprises the hydrogen and the rest part of the monosilane, and the temperature of the liquid products is 65 ℃ below zero to 85 ℃ below zero;
D) introducing the liquid product into the light component removal separation tower for rectification and purification, collecting gaseous monosilane from the tower top of the light component removal separation tower, and discharging the liquid product without the monosilane from the tower bottom of the light component removal separation tower, wherein the pressure in the light component removal separation tower is between 0.4MPaG and 0.6MpaG, and the temperature in the light component removal separation tower is between 32 ℃ and 50 ℃;
E) introducing the liquid product from which the monosilane is separated into the adsorption device so that an adsorbent in the adsorption device can adsorb metal impurities in the liquid product;
F) and introducing the liquid product without the metal impurities into the de-heavy separation tower for rectification and purification so as to separate high-order silane in the liquid product without the metal impurities and obtain disilane, wherein the pressure in the de-heavy separation tower is between 0.05MPaG and 0.4MpaG, and the temperature in the de-heavy separation tower is between-4 ℃ and 37 ℃.
In some embodiments, the step a) further comprises:
and filtering the heated monosilane by using the first precision filter so as to remove the microsilica in the heated monosilane.
In some embodiments, said step B) comprises:
b-1) filtering the mixed reaction gas by using the second precision filter so as to remove the micro silicon powder in the mixed reaction gas;
b-2) carrying out first heat exchange on the mixed reaction gas by using the first preheater so as to reduce the temperature of the mixed reaction gas;
b-3) pressurizing the mixed reaction gas by a compressor so as to obtain a pressurized mixed reaction gas, wherein the pressure of the pressurized mixed reaction gas is between 0.5MPaG and 1.5MpaG, and optionally the pressure of the pressurized mixed reaction gas is between 0.6MPaG and 0.8 MpaG;
b-4) carrying out secondary heat exchange on the pressurized mixed reaction gas and the monosilane in the produced gas state by using the second preheater so as to reduce the temperature of the pressurized mixed reaction gas and increase the temperature of the monosilane in the produced gas state.
In some embodiments, the monosilane in the produced gas state is passed into the heating device as a feedstock.
Drawings
FIG. 1 is a schematic structural view of a disilane production apparatus according to an embodiment of the invention.
FIG. 2 is a schematic structural view of a disilane production apparatus according to an embodiment of the invention.
FIG. 3 is a schematic structural view of a disilane production apparatus according to an embodiment of the invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
A disilane production apparatus 1000 according to an embodiment of the present invention will be described below with reference to the drawings. As shown in fig. 1 to 3, a disilane production apparatus 1000 according to an embodiment of the present invention includes a heating device 100, a catalytic dehydrogenation reactor 200, a cryogenic device 300, a light ends removal separation column 400, an adsorption device 500, and a heavy ends removal separation column 600.
The heating device 100 has a first air inlet 110 and a first air outlet 120. The catalytic dehydrogenation reactor 200 has a second gas inlet 210 and a second gas outlet 220, the second gas inlet 210 being in communication with the first gas outlet 120. The cryogenic device 300 is provided with a third air inlet 310, a third liquid outlet 320 and a third waste gas outlet 330, wherein the third air inlet 310 is communicated with the second air outlet 220;
the light component removal separation column 400 has a fourth feed port 410, a fourth gas outlet 420 and a fourth liquid outlet 430, the fourth feed port 410 is communicated with the third liquid outlet 320, and the fourth gas outlet 420 is communicated with the first gas inlet 110. The adsorption device 500 has a fifth inlet 510 and a fifth outlet 520, and the fifth inlet 510 is communicated with the fourth outlet 430. The separation column 600 has a sixth inlet 610, a sixth outlet 620 and a sixth outlet 630, and the sixth inlet 610 is communicated with the fifth outlet 520.
In the related art, disilane is generally produced by a direct silane synthesis method, in which monosilane is used as a starting material and is converted into disilane by atomic excitation, thermal decomposition, photolysis, electrostatic field, glow discharge, and the like. However, the method has low conversion rate, brown yellow amorphous silicon solid substances are easily generated in the process, and the industrial application value is not high.
The disilane production apparatus 1000 according to the embodiment of the invention performs a catalytic dehydrogenation reaction on monosilane using the catalytic dehydrogenation reactor 200, thereby generating a mixed reaction gas including disilane. The monosilane is generated into the disilane by the catalytic method only by the catalyst and at a certain temperature, so the environment required by the catalytic reaction is easily achieved, the arrangement of the catalytic dehydrogenation reactor 200 is easily completed, the manufacturing difficulty of the disilane preparation equipment 1000 is reduced, and the process of generating the disilane by the catalytic method is simpler. The impurity species in the mixed reaction gas are few, and other substances except disilane in the mixed reaction gas are convenient to separate and remove, namely, the disilane preparation equipment 1000 is high in conversion rate and production efficiency by using monosilane as a raw material to prepare disilane.
The mixed reaction gas comprises disilane, hydrogen, higher-order silane and monosilane, the hydrogen can be separated by using the deep cooling device 300, the monosilane can be separated by using the light component removal separation tower 400, and the higher-order silane can be separated by using the heavy component removal separation tower 600. The hydrogen and the high-order silane belong to raw materials with recovery value, the monosilane can be continuously used as production raw materials, and the waste of resources and the production cost can be reduced by recovering the hydrogen, the high-order silane and the monosilane.
Therefore, the disilane preparing apparatus 1000 according to the embodiment of the invention has the advantages of high disilane conversion rate, high production efficiency, reduced resource waste, reduced production cost, and the like.
A method of preparing disilane according to an embodiment of the invention includes the steps of:
A) the monosilane is heated by the heating apparatus 100 so that the temperature of the monosilane is heated to 100 ℃ to 250 ℃.
B) Introducing the heated monosilane into a catalytic dehydrogenation reactor 200 to perform catalytic dehydrogenation reaction so as to obtain mixed reaction gas, wherein the mixed reaction gas comprises disilane, hydrogen, higher-order silane and monosilane, and the catalytic dehydrogenation reaction is performed at the temperature of 100-250 ℃ and under the condition of 0.2MPaG-0.4 MpaG.
C) The mixed reaction gas is cooled by using the deep cooling device 300 so as to obtain non-condensable gas and liquid products, wherein the liquid products comprise one part of monosilane, disilane and high-order silane, the non-condensable gas comprises hydrogen and the rest part of monosilane, and the temperature of the liquid products is 65 ℃ below zero-85 ℃.
D) Introducing the liquid product into a light component removal separation tower 400 for rectification and purification, collecting gaseous monosilane from the top of the light component removal separation tower 400, and discharging liquid product without monosilane from the bottom of the light component removal separation tower 400, wherein the pressure in the light component removal separation tower 400 is between 0.4MPaG and 0.6MpaG, and the temperature in the light component removal separation tower 400 is between 32 and 50 ℃.
E) The liquid product from which monosilane is separated is introduced into the adsorption device 500, so that the adsorbent in the adsorption device 500 adsorbs the metal impurities in the liquid product.
F) And introducing the liquid product without the metal impurities into a de-heavy separation tower 600 for rectification and purification so as to remove high-order silane in the liquid product without the metal impurities and obtain disilane, wherein the pressure in the de-heavy separation tower 600 is between 0.05MPaG and 0.4MpaG, and the temperature in the de-heavy separation tower 600 is between-4 ℃ and 37 ℃.
The disilane preparation method according to the embodiment of the invention performs a catalytic dehydrogenation reaction on monosilane using the catalytic dehydrogenation reactor 200, thereby generating a mixed reaction gas including disilane. The process of using the catalysis method to generate the disilane by the silane is simple, the impurity types in the mixed reaction gas are few, and other substances except the disilane in the mixed reaction gas are convenient to separate and remove, namely, the disilane is prepared by using the disilane as a raw material by the disilane preparation equipment 1000, so that the conversion rate is high, and the production efficiency is high.
The mixed reaction gas comprises disilane, hydrogen, higher-order silane and monosilane, the hydrogen can be separated by using the deep cooling device 300, the monosilane can be separated by using the light component removal separation tower 400, and the higher-order silane can be separated by using the heavy component removal separation tower 600. The hydrogen and the high-order silane belong to raw materials with recovery value, the monosilane can be continuously used as production raw materials, and the waste of resources and the production cost can be reduced by recovering the hydrogen, the high-order silane and the monosilane.
Therefore, the disilane preparation method provided by the embodiment of the invention has the advantages of high disilane conversion rate, high production efficiency, reduction of resource waste, reduction of production cost and the like.
The disilane production method according to the embodiment of the invention may be implemented by the disilane production apparatus 1000 according to the embodiment of the invention.
As shown in fig. 1 to 3, a disilane production apparatus 1000 according to an embodiment of the present invention includes a heating device 100, a first precision filter 810, a catalytic dehydrogenation reactor 200, a second precision filter 820, a compressor 700, a cryogenic device 300, a first preheater 910, a second preheater 920, a light ends separation column 400, an adsorption device 500, and a heavy ends separation column 600.
The heating device 100 has a first air inlet 110 and a first air outlet 120. Monosilane enters the heating device 100 from the first gas inlet 110 to be heated, so that the temperature of the monosilane is heated to 100-250 ℃. The heated monosilane, after reaching the temperature required for the catalytic dehydrogenation reaction, is discharged out of the heating apparatus 100 through the first gas outlet 120.
The first precision filter 810 has a first filtered inlet 811 and a first filtered outlet 812. The first filtered inlet 811 is connected to the first outlet port 120 and the first filtered outlet 812 is connected to the second inlet port 210. The first fine filter 810 plays a role in gas-solid separation, solid impurities (micro silicon powder) can be generated by thermal decomposition of the silane due to high local temperature during heating, so that the heated silane enters the first fine filter 810 through the first filtering outlet 812 for filtering, and after the solid impurities in the heated silane are filtered, the heated silane is discharged out of the first fine filter 810 through the first filtering outlet 812.
As shown in fig. 2, in some embodiments, catalytic dehydrogenation reactor 200 has a second gas inlet 210 and a second gas outlet 220, with second gas inlet 210 communicating with first gas outlet 120. The heated monosilane exiting the first filtered outlet 812 enters the catalytic dehydrogenation reactor 200 by entering the second inlet 210. The heated monosilane undergoes a catalytic dehydrogenation reaction in the catalytic dehydrogenation reactor 200 to obtain a mixed reaction gas, which includes disilane, hydrogen, higher-order silane, and monosilane. The monosilane in the mixed reaction gas comprises unreacted monosilane and monosilane generated by the reaction of disilane and trisilane with hydrogen.
The catalytic dehydrogenation reaction is carried out at 100-250 ℃ and under the condition of 0.2MPaG-0.4MpaG, so that the reaction efficiency is accelerated, a large amount of thermal decomposition of monosilane caused by overheating is avoided, the production of disilane can be ensured, and the production efficiency is ensured.
The catalytic dehydrogenation reactor 200 is a tubular reactor, which can effectively avoid material back-mixing. The catalytic dehydrogenation reactor 200 is filled with a catalyst and a gas distributor, and a porous carrier is arranged in the catalytic dehydrogenation reactor 200, so that the catalyst can be loaded on the porous carrier, the distribution of the catalyst is uniform, and the catalyst is convenient to contact with gas. The gas distributor enables the heated monosilane to uniformly enter the catalyst bed layer for reaction, and ensures the rapid proceeding of the catalytic dehydrogenation reaction.
Optionally, the porous support comprises activated carbon, alumina and molecular sieves. Optionally, the catalyst comprises at least one of oxides of zinc, nickel, iron, copper.
In some embodiments, second precision filter 820 has a second filtered inlet 821 and a second filtered outlet 822. Second filtered inlet 821 is coupled to second outlet 220 and second filtered outlet 822 is coupled to seventh inlet 710.
The mixed reaction gas is discharged from the second gas outlet 220 out of the catalytic dehydrogenation reactor 200, and enters the second precision filter 820 through the second filtering inlet 821, so as to remove a small amount of silicon micropowder generated by thermal decomposition of monosilane in the catalytic dehydrogenation reactor 200. The mixed gas after removing the impurities is discharged out of the second precision filter 820 through the second filtering outlet 822.
As shown in FIG. 2, in some embodiments, the compressor 700 has a seventh inlet 710 and a seventh outlet 720, the seventh inlet 710 is connected to the second outlet 220, and the seventh outlet 720 is in communication with the third inlet 310. The mixed gas from which the impurities are removed is pressurized through the seventh gas inlet 710, and the pressurized mixed gas is discharged out of the compressor 700 through the seventh gas outlet 720. The pressure of the pressurized mixed gas is between 0.5MPaG and 1.5 MpaG. The mixed gas is pressurized to provide original power for the material, so that the mixed gas has higher pressure, and the mixed gas can form pressure gradient along the process flow of the system. The mixed gas is transmitted by means of pressure gradient, so that the use of secondary pressurizing equipment such as a pump is avoided, the equipment investment is reduced, and the safety of the equipment is improved.
Optionally, the pressure of the pressurized mixed gas is between 0.6MPaG and 0.8 MpaG.
The cryogenic device 300 has a third gas inlet 310, a third liquid outlet 320 and a third waste gas outlet 330, wherein the third gas inlet 310 is communicated with the second gas outlet 220. The pressurized mixed reactant gas is cooled in cryogenic device 300 through third gas inlet 310 to obtain non-condensable gases and liquid products. The liquid product comprises a part of monosilane, disilane and higher-order silane, and the temperature of the liquid product is minus 65 ℃ to minus 85 ℃. The non-condensable gas comprises hydrogen and the rest of the monosilane, and only a small amount of monosilane is contained in the non-condensable gas. Non-condensable gases are discharged from cryogenic device 300 through third waste gas outlet 330 and liquid product is discharged from cryogenic device 300 through third liquid outlet 320.
As shown in fig. 3, the lightness-removing separating column 400 has a fourth feed opening 410, a fourth gas outlet 420 and a fourth liquid outlet 430, the fourth feed opening 410 is communicated with the third liquid outlet 320, and the fourth gas outlet 420 is communicated with the first gas inlet 110. The liquid product enters the light component removal separation column 400 through the fourth feed inlet 410 for rectification and purification. The light component removal separation tower 400 is a stainless steel packed tower. The number of trays of the light ends removal separation column 400 is between 10 and 30. The pressure in the light component removing and separating tower 400 is between 0.4MPaG and 0.6MpaG, and the temperature in the light component removing and separating tower 400 is between 32 ℃ and 50 ℃. The liquid product is rectified and purified in the light component removal and separation column 400, so that monosilane is changed from liquid to gas, and is extracted from a fourth gas outlet 420 at the top of the light component removal and separation column 400. The liquid product without monosilane is discharged from the light ends removal column 400 through a fourth liquid outlet 430 at the bottom of the column.
As shown in fig. 3, the adsorption apparatus 500 has a fifth inlet 510 and a fifth outlet 520, and the fifth inlet 510 is communicated with the fourth outlet 430. The liquid product from which monosilane is separated is introduced into the adsorption device 500 through the fifth feed port 510, so that the metal impurities in the liquid product are adsorbed by the adsorbent in the adsorption device 500. The pressure in the adsorption unit 500 is between 0.1MPaG and 0.5MPaG so that the liquid product from which monosilane is separated can flow into the adsorption unit 500 by itself.
Alternatively, the pressure within the adsorption device 500 is between 0.2MPaG and 0.4 MpaG.
As shown in fig. 3, the de-weight separation column 600 has a sixth inlet 610, a sixth outlet 620 and a sixth outlet 630, and the sixth inlet 610 is communicated with the fifth outlet 520. The liquid product without metal impurities is fed into the de-heavy separation column 600 through the sixth feed port 610 for rectification and purification. The de-weighting separation tower 600 is a stainless steel packing tower, and the number of tower plates of the de-weighting separation tower 600 is between 20 and 40. The pressure in the de-heavy separation tower 600 is between 0.05MPaG and 0.4MpaG, and the temperature in the de-heavy separation tower 600 is between-4 ℃ and 37 ℃. Disilane in the liquid product from which the metal impurities are removed is changed from liquid to gas in the de-heavy separation tower 600, and is extracted and collected from a sixth gas outlet 620 at the top of the tower. The higher-order silanes (high-boiling substances) in the liquid product from which the metal impurities are removed are discharged from the de-heavy separation column 600 through a sixth liquid outlet 630 at the bottom of the column.
Alternatively, the pressure within the de-heavy separation column 600 is between 0.1MPaG and 0.25 MPaG. The pressure within the adsorption unit 500 is between 0.2MPaG and 0.4 MPaG.
In some embodiments, the pressure within the light ends separation column 400, the adsorption unit 500, and the de-heavy separation column 600 is sequentially reduced, and the pressure difference between the light ends separation column 400, the adsorption unit 500, and the de-heavy separation column 600 is 0.2 MPaG. The pressure difference among the light component removal separation tower 400, the adsorption device 500 and the heavy component removal separation tower 600 can be utilized to transmit materials, the use of devices such as a conveying pump and the like can be reduced, the safety of the system is improved, and the operation cost and the equipment investment are reduced.
As shown in fig. 2, in some embodiments, a disilane production apparatus 1000 according to embodiments of the invention further comprises a first preheater 910 and a second preheater 920.
The first preheater 910 includes a first heating cavity and a first cooling cavity, and the first heating cavity and the first cooling cavity are mutually matched, so that the gas in the first heating cavity and the gas in the first cooling cavity can exchange heat. The first heating chamber has a first heating inlet 911 and a first heating outlet 912, the first cooling chamber has a first cooling inlet 913 and a first cooling outlet 914, the first heating outlet 912 is connected to the first inlet 110, the first cooling inlet 913 is connected to the second filtering outlet 822, and the first cooling outlet 914 is connected to the seventh inlet 710.
Raw material monosilane enters a first heating cavity in the first preheater 910 through a first heating inlet 911, and mixed reaction gas enters a first cooling cavity through a first cooling inlet 913. The raw material monosilane exchanges heat with the mixed reaction gas in the first cooling cavity for the first time, so that the temperature of the monosilane is increased, and the temperature of the mixed reaction gas is reduced. The cooled mixed reactant gas is discharged through the first cooling outlet 914 and then enters the compressor 700 through the seventh inlet 710. The increased-temperature monosilane is discharged through the first heating outlet 912, and then enters the heating apparatus 100 through the first inlet 110.
The second preheater 920 includes a second heating cavity and a second cooling cavity, and the second heating cavity and the second cooling cavity are mutually matched, so that the gas in the second heating cavity and the gas in the second cooling cavity can exchange heat. The second heating chamber has a second heating inlet 921 and a second heating outlet 922, and the second cooling chamber has a second cooling inlet 923 and a second cooling outlet 924. The second cooling inlet 923 is connected to the seventh outlet 720, the second cooling outlet 924 is connected to the third inlet 310, the second heating inlet 921 is connected to the fourth outlet 420, and the second heating outlet 922 is connected to the first heating inlet 911.
Monosilane extracted from the top of the light component removal separation tower 400 enters the second heating cavity through the second heating inlet 921, and the pressurized mixed reaction gas enters the second cooling cavity through the second cooling inlet 923. The extracted monosilane is subjected to a second heat exchange with the pressurized mixed reaction gas to lower the temperature of the pressurized mixed reaction gas and to raise the temperature of the extracted gaseous monosilane. The reduced temperature pressurized mixed reactant gas exits through second cooling outlet 924 and enters cryogenic device 300 through third inlet 310. The gaseous extracted monosilane having an increased temperature is used as a raw material, and after being discharged through the second heating outlet 922, the gaseous extracted monosilane enters the first heating cavity of the first preheater 910 through the first heating inlet 911.
The first preheater 910 and the second preheater 920 facilitate energy recovery and utilization, reduce energy consumption of the disilane production apparatus 1000, and reduce operation cost.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through an intermediate. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the present disclosure, the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" and the like mean that a specific feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present disclosure. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A disilane production apparatus, comprising:
a heating device having a first air inlet and a first air outlet;
the catalytic dehydrogenation reactor is provided with a second gas inlet and a second gas outlet, and the second gas inlet is communicated with the first gas outlet;
the cryogenic device is provided with a third air inlet, a third liquid outlet and a third waste gas outlet, and the third air inlet is communicated with the second air outlet;
the light component removing and separating tower is provided with a fourth feeding hole, a fourth gas outlet and a fourth liquid outlet, the fourth feeding hole is communicated with the third liquid outlet, and the fourth gas outlet is communicated with the first gas inlet;
the adsorption device is provided with a fifth feeding hole and a fifth discharging hole, and the fifth feeding hole is communicated with the fourth liquid outlet; and
and the de-weight separation tower is provided with a sixth feeding hole, a sixth gas outlet and a sixth liquid outlet, and the sixth feeding hole is communicated with the fifth discharging hole.
2. The disilane production apparatus according to claim 1, further comprising a compressor having a seventh inlet port and a seventh outlet port, said seventh inlet port being connected to said second outlet port, said seventh outlet port being in communication with said third inlet port.
3. The disilane production apparatus according to claim 2, further comprising:
a first precision filter having a first filter inlet and a first filter outlet, the first filter inlet being connected to the first gas outlet, the first filter outlet being connected to the second gas inlet; and
and the second precision filter is provided with a second filtering inlet and a second filtering outlet, the second filtering inlet is connected with the second air outlet, and the second filtering outlet is connected with the seventh air inlet.
4. The disilane production apparatus according to claim 3, further comprising:
the first preheater comprises a first heating cavity and a first cooling cavity, the first heating cavity is matched with the first cooling cavity, the first heating cavity is provided with a first heating inlet and a first heating outlet, the first cooling cavity is provided with a first cooling inlet and a first cooling outlet, the first heating outlet is connected with the first air inlet, the first cooling inlet is connected with the second filtering outlet, and the first cooling outlet is connected with the seventh air inlet; and
the second preheater comprises a second heating cavity and a second cooling cavity, the second heating cavity is matched with the second cooling cavity, the second heating cavity is provided with a second heating inlet and a second heating outlet, the second cooling cavity is provided with a second cooling inlet and a second cooling outlet, the second cooling inlet is connected with the seventh gas outlet, the second cooling outlet is connected with the third gas inlet, the second heating inlet is connected with the fourth gas outlet, and the second heating outlet is connected with the first heating inlet.
5. The disilane production plant of claim 1, wherein the catalytic dehydrogenation reactor is a tubular reactor, and wherein the catalytic dehydrogenation reactor is loaded with a catalyst, optionally wherein the catalyst comprises at least one of oxides of zinc, nickel, iron, and copper.
6. The disilane production apparatus of claim 1, wherein a porous support is disposed within the catalytic dehydrogenation reactor, optionally wherein the porous support comprises activated carbon, alumina, and molecular sieves.
7. A disilane production method performed by the disilane production apparatus according to any one of claims 1-6, comprising the steps of:
A) heating monosilane by using the heating device so as to heat the temperature of the monosilane to 100-250 ℃;
B) introducing the heated monosilane into the catalytic dehydrogenation reactor to perform catalytic dehydrogenation reaction so as to obtain mixed reaction gas, wherein the mixed reaction gas comprises disilane, hydrogen, higher-order silane and monosilane, and the catalytic dehydrogenation reaction is performed at the temperature of 100-250 ℃ and under the condition of 0.2MPaG-0.4 MpaG;
C) cooling the mixed reaction gas by using the cryogenic device so as to obtain non-condensable gas and liquid products, wherein the liquid products comprise one part of the monosilane, the disilane and the high-order silane, the non-condensable gas comprises the hydrogen and the rest part of the monosilane, and the temperature of the liquid products is 65 ℃ below zero to 85 ℃ below zero;
D) introducing the liquid product into the light component removal separation tower for rectification and purification, collecting gaseous monosilane from the tower top of the light component removal separation tower, and discharging the liquid product without the monosilane from the tower bottom of the light component removal separation tower, wherein the pressure in the light component removal separation tower is between 0.4MPaG and 0.6MpaG, and the temperature in the light component removal separation tower is between 32 ℃ and 50 ℃;
E) introducing the liquid product from which the monosilane is separated into the adsorption device so that an adsorbent in the adsorption device can adsorb metal impurities in the liquid product;
F) and introducing the liquid product without the metal impurities into the de-heavy separation tower for rectification and purification so as to separate high-order silane in the liquid product without the metal impurities and obtain disilane, wherein the pressure in the de-heavy separation tower is between 0.05MPaG and 0.4MpaG, and the temperature in the de-heavy separation tower is between-4 ℃ and 37 ℃.
8. The method of claim 7, wherein step a) further comprises:
and filtering the heated monosilane by using the first precision filter so as to remove the microsilica in the heated monosilane.
9. The method of claim 7, wherein step B) comprises:
b-1) filtering the mixed reaction gas by using the second precision filter so as to remove the micro silicon powder in the mixed reaction gas;
b-2) carrying out first heat exchange on the mixed reaction gas by using the first preheater so as to reduce the temperature of the mixed reaction gas;
b-3) pressurizing the mixed reaction gas by a compressor so as to obtain a pressurized mixed reaction gas, wherein the pressure of the pressurized mixed reaction gas is between 0.5MPaG and 1.5MpaG, and optionally the pressure of the pressurized mixed reaction gas is between 0.6MPaG and 0.8 MpaG;
b-4) carrying out secondary heat exchange on the pressurized mixed reaction gas and the monosilane in the produced gas state by using the second preheater so as to reduce the temperature of the pressurized mixed reaction gas and increase the temperature of the monosilane in the produced gas state.
10. The method according to claim 7, wherein the monosilane in the produced gas state is introduced into the heating device as a raw material.
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| CN114314596A (en) * | 2021-12-01 | 2022-04-12 | 全椒亚格泰电子新材料科技有限公司 | Method and system for continuously synthesizing high-order silane by utilizing microwave heating fixed bed |
| CN114715900A (en) * | 2022-05-18 | 2022-07-08 | 北京化工大学 | Continuous production preparation system and production process of electronic-grade disilane |
| CN115403048A (en) * | 2022-10-13 | 2022-11-29 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for purifying disilane |
| CN115477305A (en) * | 2022-10-19 | 2022-12-16 | 浙江中宁硅业有限公司 | Disilane and preparation method thereof |
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