CN107311183A - A kind of method and device of hydrogen plasma method synthesizing silane - Google Patents
A kind of method and device of hydrogen plasma method synthesizing silane Download PDFInfo
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- CN107311183A CN107311183A CN201710767288.9A CN201710767288A CN107311183A CN 107311183 A CN107311183 A CN 107311183A CN 201710767288 A CN201710767288 A CN 201710767288A CN 107311183 A CN107311183 A CN 107311183A
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- 229910000077 silane Inorganic materials 0.000 title claims abstract description 161
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 239000001257 hydrogen Substances 0.000 title claims abstract description 140
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 140
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 238000000034 method Methods 0.000 title claims abstract description 69
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000007789 gas Substances 0.000 claims abstract description 75
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 44
- 235000013312 flour Nutrition 0.000 claims abstract description 39
- 238000013461 design Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 146
- 210000002381 plasma Anatomy 0.000 claims description 88
- 230000015572 biosynthetic process Effects 0.000 claims description 64
- 238000003786 synthesis reaction Methods 0.000 claims description 64
- 239000008246 gaseous mixture Substances 0.000 claims description 35
- 239000010703 silicon Substances 0.000 claims description 31
- 229910052710 silicon Inorganic materials 0.000 claims description 31
- 239000005049 silicon tetrachloride Substances 0.000 claims description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 30
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 19
- 239000002826 coolant Substances 0.000 claims description 14
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 239000007921 spray Substances 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- -1 silicon Alkane Chemical class 0.000 claims description 5
- 238000009834 vaporization Methods 0.000 claims description 5
- 230000008016 vaporization Effects 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 238000010891 electric arc Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 2
- 239000000110 cooling liquid Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 17
- 230000008569 process Effects 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 238000010189 synthetic method Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000002955 isolation Methods 0.000 abstract description 3
- 238000011109 contamination Methods 0.000 abstract description 2
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 abstract 1
- 210000004483 pasc Anatomy 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 12
- 238000003860 storage Methods 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 238000011084 recovery Methods 0.000 description 9
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 8
- 239000005052 trichlorosilane Substances 0.000 description 8
- 238000012850 discrimination method Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000003507 refrigerant Substances 0.000 description 6
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229910007981 Si-Mg Inorganic materials 0.000 description 3
- 229910008316 Si—Mg Inorganic materials 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000000149 penetrating effect Effects 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 229910021338 magnesium silicide Inorganic materials 0.000 description 2
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical group Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- 239000012448 Lithium borohydride Substances 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910019752 Mg2Si Inorganic materials 0.000 description 1
- 229910020828 NaAlH4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000019628 coolness Nutrition 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000012280 lithium aluminium hydride Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
-
- 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
- C01B33/043—Monosilane
Abstract
The invention discloses a kind of method of hydrogen plasma method synthesizing silane, this is ionized silica flour using hydrogen plasma generator, hydrogen after ionization generates silane with pasc reaction, mixed gas separation system is introduced after by silane and hydrogen mixed gas chilling, so as to obtain silane, and the hydrogen after separating is recycled.The process employs ripe hydrogen plasma technology, chilling technique and silane and hydrogen isolation technics, with technological process is short, small investment, energy consumption it is low, participate in reacting without others chemical substances, environmental pollution is small or substantially free of contamination advantage.And in order to preferably realize above-mentioned synthetic method, present invention also offers a kind of device of hydrogen plasma method synthesizing silane --- silane synthetic tower, the synthetic tower is reasonable in design, and compact conformation, floor space is small, and synthetic effect is good.
Description
Technical field
The present invention relates to a kind of method and device of hydrogen plasma method synthesizing silane.
Background technology
Silane has a variety of preparation methods, and the production technology of current main flow has following several：
(1) magnesium silicide method：The mixed-powder of silicon and magnesium is reacted in about 500 DEG C of hydrogen, the magnesium silicide of generation and
Ammonium chloride reacts in low temperature liquid ammonia, can obtain silane.It can obtain after it is refined in the distilling apparatus cooled down with liquid nitrogen
Pure silane.
(2) discrimination method：Si powder, silicon tetrachloride and hydrogen are reacted in the fluidized-bed furnace being heated to more than 500 DEG C, obtained
Trichlorosilane.Trichlorosilane is separated with the way of distillation.Reacted in the presence of a catalyst by not being homogenized.To dichlorosilane.Gained
Dichlorosilane be mixture with silicon tetrachloride, trichlorosilane, so with the way of distillation it is refined after pure dichlorosilane.Using not
Homogenizing catalysts obtain trichlorosilane and single silane by dichlorosilane.The single silane of gained is carried with cryogenic high pressure distilling apparatus
It is pure.
(3) HCl treatment Si-Mg alloy is used.
Mg2Si+4HCl—→2MgCl2+SiH4
(4) Si-Mg alloy reacts with ammonium bromide in liquefied ammonia.
(5) using lithium aluminium hydride reduction, lithium borohydride etc. as reducing agent, tetrachloro silicane or trichlorosilane are reduced in ether.
The common feature of above-mentioned five kinds of methods is that flow is complicated, has other metallicses or chemical substance to be carried as centre
Body, easily produces otherwise environmental issue, and also has investment cost big, and high energy consumption, processing medium purification difficulty is big
The problems such as.
Wherein acceptance highest is the technology that discrimination method produces silane, mass produces the method for silane substantially at present
Using this technology.But the greatest problem of this technology is technological process length, conversion ratio is low, internal circulating load is big, high energy consumption, have dirt
Dye, not only consumption of raw material is big, also needs substantial amounts of chemicals to neutralize waste liquid, the waste liquid and waste residue amount of product are very big.
The content of the invention
The invention aims to solve above-mentioned technical problem, there is provided a kind of dress of hydrogen plasma method synthesizing silane
Put --- silane synthetic tower, the synthetic tower is reasonable in design, and compact conformation, floor space is small, and synthetic effect is good.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of device of hydrogen plasma method synthesizing silane, including housing and plasma generator；From upper past in the housing
Under be set to plasma generating region, silane synthesis zone, Pen Qing chillings area, hydrojet chilling area and gas-liquid separation zone successively, and silane is closed
Into being additionally provided with the synthesis tail gas outlet that internal diameter gradually increases from top to bottom between area and Pen Qing chillings area；The plasma generator
Negative pole is upward, positive pole is directed downwardly is arranged in plasma generating region, and the plasma generating region side is provided with raw hydrogen entrance；
The silane synthesis zone side is provided with raw material particulate silicon inlet；The Pen Qing chillings area side is uniformly provided with some cold conditions hydrogen and sprayed into
Mouthful；The hydrojet chilling area bottom sides are provided with multiple cold liquid entrances, and hydrojet chilling area inner homogeneous is provided with multigroup sparge pipe, and
Some nozzles are uniformly provided with every group of sparge pipe, the entrance of sparge pipe is connected with cold night entrance；The gas-liquid separation zone side
Top is provided with below syngas outlet, gas-liquid separation zone and is set to liquid outlet.
Specifically, the longitudinal section of the gas-liquid separation zone is in convex shape, and the syngas outlet is in inverted L-shaped, and is synthesized
Gas exports the top for being arranged on gas-liquid separation zone lateral spine.
Specifically, hydrojet collecting region and solid-liquid mixed collection are also sequentially provided with below gas-liquid separation zone in the housing
Area；The hydrojet collecting region is in reverse frustoconic structure, and hydrojet collecting region side middle and upper part is provided with liquid outlet；The solid-liquid is mixed
Close collecting region bottom and be provided with the first solid-liquid outlet.
In particular, the liquid outlet is horizontally disposed with, and liquid outlet is provided with the second downward solid-liquid outlet,
Liquid outlet end picks out pipe provided with an inverted U-shaped liquid；The second solid-liquid outlet is higher than the hydrojet collecting region bottom,
The liquid picks out pipe highest point less than syngas outlet bottom, and liquid is picked out at the top of pipe lowest part hydrojet collecting region.
Another object of the present invention be then to provide for it is a kind of using above-mentioned silane synthetic tower come the method for synthesizing silane,
This method combines ripe hydrogen plasma technology, chilling technique and silane and hydrogen isolation technics carrys out synthesizing silane, technological process is short,
Small investment, energy consumption are low, participate in reaction without others chemical substance, environmental pollution is small or substantially pollution-free.
To achieve the above object, the technical solution adopted by the present invention is as follows：
It is a kind of using above-mentioned silane synthetic tower come the method for synthesizing silane, excessive hydrogen and silica flour are passed through hydrogen plasma
In the device of method synthesizing silane, plasma generator is by silica flour and excessive hydrogen ionization, and the hydrogen and silicon after ionization are abundant
Haptoreaction, obtains the synthesis tail gas being mainly made up of silane and hydrogen, then by synthesis tail gas elder generation and hydrogen mixing chilling, obtain
Chilling is mixed with coolant to gaseous mixture, then by gaseous mixture, finally again separates gaseous mixture with coolant, you can is obtained comprising conjunction
Into the gaseous mixture of silane.
Specifically, the synthetic method comprises the following steps：
The A preparatory stages：The gas in the device of hydrogen plasma method synthesizing silane is all first replaced into hydrogen, is then turned on closing
Into gas outlet, cold conditions hydrogen entrance, cold liquid entrance, to hydrojet collecting region in liquid level reach design liquid level after, start plasma
Generator, makes plasma generating region produce electric arc；
B plasmas：Open raw hydrogen entrance, hydrogen with pressure be heated rapidly by plasma generating region and by from
After sonization, into silane synthesis zone；
C is synthesized：Raw material particulate silicon inlet is opened, silica flour is passed through into silane synthesis zone, the silica flour into silane synthesis zone is fast
The high-temperature fusion of the plasma of fast quilt, vaporize to plasma, be the hydrogen and silicon synthesizing silane of plasma shape, synthesized
Tail gas, obtained synthesis tail gas temperature is 4000~6000K；
D is cooled down for the first time：Synthesis tail gas enters Pen Qing chillings area, normal temperature hydrogen and the synthesis of penetrating by synthesis tail gas outlet
Tail gas is mixed, and synthesis tail gas is cooled to less than 800 DEG C, also, synthesis tail gas is mixed to form gaseous mixture with hydrogen；
E is cooled down again：Gaseous mixture down into hydrojet chilling area, in the hydrojet chilling area by coolant by sparge pipe and
After nozzle sprays, form cold atomization area, gaseous mixture can be completed after entering with atomized liquid coolant in the area it is cold and hot exchange, make mixing
Gas is cooled to less than 30 DEG C；
F gas-liquid separations：Above-mentioned gaseous mixture and coolant enter gas-liquid separation zone together, and gaseous mixture is arranged from syngas outlet
Go out, and remaining liquid is then discharged by gas-liquid separation zone bottom.
Further, in the step, the remaining liquid by behind the bottom of gas-liquid separation zone enter hydrojet collecting region,
Enter back into liquid outlet and pick out pipe discharge via liquid.
Further, in the step, after gaseous mixture is handled through pressure-variable adsorption, silane and hydrogen partial are adsorbed, trip
From hydrogen discharge；Hydrogen after discharge enters hydrogen-holder, then after being pressurized through hydrogen gas compressor, gives plasma generator to supply respectively
Hydrogen, and Pen Qing chillings area hydrogen supply is given after can cooling down；Enter separator after silane and hydrogen desorption after absorption, through deep cooling, by gas
The silane of state is changed into liquid silane, and hydrogen is then discharged into above-mentioned hydrogen-holder at the top of separator and circulated；Liquid-state silicon
Alkane is discharged in the middle part of separator, into silane wet tank.
It is preferred that, the silica flour particle diameter is less than 0.1mm.
It is preferred that, the coolant is liquid silicon tetrachloride, and the silicon tetrachloride temperature is -10 DEG C~5 DEG C.
Compared with prior art, the invention has the advantages that：
(1) silane synthetic tower collection silica flour of the invention and plasma hydrogen reactor, spray hydrogen quencher, hydrojet quencher,
(gas, liquid, solid) separator is in one, and its is reasonable in design, and integrated level is high, and compact conformation, floor space is small, operates more convenient and closes
It is good into effect.Also, the equipment is applied in the production technology of hydrogen Plasma synthesis silane, can substantially reduce project construction into
Sheet and production cost, save project land used, and energy consumption is low, environmental protection.
(2) high temperature that the present invention is produced using plasma, hydrogen and silica flour are ionized, the activity of hydrogen and silicon is improved,
Generation silane is combined in ionic condition hydrogen and silicon, using hydrogen plasma method synthesizing silane technology, no chlorine production polycrystalline can be accomplished
Silicon, is the new technology for substituting improved Siemens polysilicon production process and existing process for producing silicane, with technological process
Short, small investment, energy consumption are low, and reaction is participated in without others chemical substances, and environmental pollution is small or substantially free of contamination feature.
Brief description of the drawings
Fig. 1 is silane synthetic tower structural representation of the present invention.
Fig. 2 (Fig. 2 is made up of Fig. 2 a, Fig. 2 b and Fig. 2 c) is the integrated artistic flow chart of silane synthetic method.
Wherein, reference is corresponding entitled：
101- plasmas generating region, 102- silane synthesis zones, the outlet of 103- synthesis tail gas, 104- Pen Qing chillings area, 105-
Hydrojet chilling area, 106- gas-liquid separation zones, 107- hydrojet collecting regions, 108- solid-liquid mixed collections area.
1- plasma generator negative poles, 2- plasma apparatus jacket water (J.W.)s, 3- plasma generator positive poles, 4- raw material silica flours enter
Mouthful, 5- quencher equipment jacket water (J.W.)s, 6- cold conditions hydrogen entrances, 7- sparge pipes, the cold liquid entrances of 8-, 9- syngas outlets, 10- silicon
Alkane synthetic tower segregation section, 11- liquid picks out pipe, 12- the first solid-liquid outlets, 13- the second solid-liquid outlets, the discharge of 14- liquid
Mouthful, 15- raw hydrogen entrances.
A- silica flour storage tanks, L- pressure-swing absorbers, M- silica powder drying devices, O- silica flour collecting tanks, O1- gas-solid conveyers, P- tetra-
Silicon chloride vaporizer, Q- silicon tetrachlorides cooling device, R- silicon tetrachlorides cooling device, S- cryogenic separators, T- hydrogen-holders, T1- hydrogen
Air compressor, V- silane wet tanks, V1- silane liquid pumps, W- silane vaporizers, X- silane gas surge tanks, X1- silane gas
Gas compressor, X2- silane gas storage tanks, Y- silicon tetrachloride storage tanks, Y1- silicon tetrachloride liquid pumps, Z- silica flour accurate filters.
Embodiment
The invention will be further described with embodiment for explanation below in conjunction with the accompanying drawings, and mode of the invention includes but not only limited
In following examples.
The silane synthetic method of the present embodiment is different from the Si-Mg alloy method that the whole world is used at present, sodium aluminum hydride (NaAlH4)
Tetrafluoride reduced (SiF4) prepare silane thermal decomposition process, the mode of production of chlorosilane discrimination method.Its topmost feature be utilize etc. from
The high temperature that daughter is produced, hydrogen and silica flour are ionized, the activity of hydrogen and silicon is improved, and generation silicon is combined in ionic condition hydrogen and silicon
Alkane.Hydrogen plasma technology, chilling technique and the silane and hydrogen isolation technics that this method is mainly applied are very ripe, can effectively contract
Flow, reduction investment, the reduction energy consumption of short whole synthesis technique, also, reaction is participated in without other chemical substances, to environment
Pollution is small or even substantially pollution-free, can be applicable.
Excessive hydrogen and silica flour are first passed through hydrogen plasma by the method for the hydrogen plasma method synthesizing silane of the present embodiment
In the device of method synthesizing silane, plasma generator is by silica flour and excessive hydrogen ionization, and the hydrogen and silicon after ionization are abundant
Haptoreaction, obtains the synthesis tail gas being mainly made up of silane and hydrogen, then by synthesis tail gas elder generation and hydrogen mixing chilling, obtain
Chilling is mixed with coolant to gaseous mixture, then by gaseous mixture, finally again separates gaseous mixture with coolant, you can is obtained comprising conjunction
Into the gaseous mixture of silane.The gaseous mixture main component is silane, hydrogen and part other impurities, by routine in the prior art
Silane mixture gas separation means, you can by mixed gas separation, obtain silane.
In order to more easily realize above-mentioned synthesis technique, the present embodiment also specially devises a kind of hydrogen plasma method synthesis silicon
Alkane device --- silane synthetic tower.
As shown in figure 1, the silane synthetic tower collection silica flour of the present embodiment and plasma hydrogen reactor, spray hydrogen quencher, hydrojet
Quencher, (gas, liquid, solid) separator are in one, and its is reasonable in design, and integrated level is high, operate more convenient.Specifically, the silane
Synthetic tower mainly includes housing and plasma generator；It is set to be cylindrical in shape or v-shaped structure successively from top to bottom in the housing
Plasma generating region 101, silane synthesis zone 102, Pen Qing chillings area 104 and hydrojet chilling area 105, and silane synthesis zone with spray
The synthesis tail gas outlet 103 that internal diameter gradually increases from top to bottom is additionally provided between hydrogen chilling area, and is also set below hydrojet chilling area
There is the gas-liquid separation zone 106 that longitudinal section is in convex shape；The plasma generator is arranged in plasma generating region 101, and is waited
Ion generator negative pole 1 is upper, and plasma generator positive pole 3 is under；The plasma generating region side enters provided with raw hydrogen
Mouth 15；The side of silane synthesis zone 102 is provided with raw material particulate silicon inlet 4；The side of Pen Qing chillings area 104 is uniformly provided with some
Cold conditions hydrogen entrance 6；The bottom sides of hydrojet chilling area 105 are provided with multiple cold liquid entrances 8, hydrojet chilling area inner homogeneous
Provided with some nozzles are uniformly provided with multigroup sparge pipe 7, and every group of sparge pipe, the entrance of sparge pipe is connected with cold night entrance；
The top of the lateral spine of gas-liquid separation zone 106 is provided with below the syngas outlet 9 of inverted L-shaped, gas-liquid separation zone also successively
Provided with hydrojet collecting region 107 and solid-liquid mixed collection area 108；The hydrojet collecting region 107 is in reverse frustoconic structure, and hydrojet is collected
Area side middle and upper part is provided with liquid outlet 14；The bottom of solid-liquid mixed collection area 108 is provided with the first solid-liquid outlet 12.
That is, gas-liquid separation zone 106, hydrojet collecting region 107 and solid-liquid mixed collection area 108 are collectively forming silane synthetic tower segregation section 10.
The liquid outlet 14 is horizontally disposed with, and liquid outlet is provided with the second downward solid-liquid outlet 13, liquid row
Outlet end picks out pipe 11 provided with an inverted U-shaped liquid；The second solid-liquid outlet 13 is higher than the bottom of hydrojet collecting region 107
Portion, the liquid picks out the highest point of pipe 11 less than the bottom of syngas outlet 9, and liquid picks out pipe lowest part hydrojet collecting region 107 and pushed up
Portion.
Due to plasma generator produce electric arc and the silicon of plasma and the temperature of hydrogen it is higher, therefore, wait from
Plasma apparatus jacket water (J.W.) 2 is equipped with sub- generating region 101, the housing of silane synthesis zone 102, and 103 are exported in synthesis tail gas
Quencher equipment jacket water (J.W.) 5 also is provided with the housing at place.
Below, it is described in detail with reference to above-mentioned silane synthetic tower come the hydrogen plasma method synthesizing silane to the present embodiment.
The whole silane synthesis and separating technology are related to set of system, and the system includes hydrogen plasma and occurs system, silicon
Powder gas-solid Transmission system, spray (hydrogen) chilling system, (silicon tetrachloride liquid refrigerants) hydrojet chilling system, (gas, liquid, solid) separation
System, (liquid, solid) separation and recovery system, liquid refrigerants cooling recirculation system, silane and hydrogen mixed gas pressure-variable adsorption segregative line
System, silane and Hydrogen cryogenic separation and recovery system, silica flour recovery system, the hydrogen pressurization circulatory system etc., the present embodiment design
System, silica flour gas-solid Transmission system, spray (hydrogen) chilling system, (silicon tetrachloride liquid are occurred for hydrogen plasma by silane synthetic tower
State refrigerant) hydrojet chilling system, (gas, liquid, solid) piece-rate system integrate, reduce the floor space of whole system, also make
It, which is operated, more facilitates.And (liquid, solid) separation and recovery system, liquid refrigerants cooling recirculation system, silane and hydrogen mixed gas become
It is existing skill to press adsorbing separation series, silane and Hydrogen cryogenic separation and recovery system, silica flour recovery system, hydrogen pressurization circulation
The routine techniques that can be used in art, therefore the equipment and its annexation that are related to it is not described in detail.
As shown in Fig. 2 being the technological process of production of hydrogen plasma method synthesizing silane below, mainly include the following steps that：
(1) preparatory stage：
First, gas displacement is carried out to whole system, it is ensured that be atmosphere of hydrogen in system；Then, syngas outlet 9 is opened
Valve, the valve of unlatching cold conditions hydrogen entrance 6, start to spray into hydrogen；The cold valve of liquid entrance 8 is then turned on, starts to spray into four chlorinations
Silicon, to hydrojet collecting region 107 in liquid level reach and be pre-designed after liquid level, start plasma generator, it is negative to plasma generator
Pole, positive pole band about 8000V voltage, make plasma generating region 101 produce electric arc；
(2) plasma：The valve of raw hydrogen entrance 15 is opened, hydrogen with pressure is electric by plasma generating region 101
After arc is heated and is ionized rapidly, into silane synthesis zone 102；
(3) synthesize：After plasma generator stable working, the valve of raw material particulate silicon inlet 4 is opened, to silane synthesis zone
It is continuous in 102 be passed through the silica flour that particle diameter is less than 0.1mm, into silica flour (and impurity in the silica flour) quilt rapidly of silane synthesis zone
The high-temperature fusion of plasma, vaporize to plasma, be the hydrogen and silicon synthesizing silane of plasma shape, obtain synthesis tail gas；
Include silane, hydrogen and slightly solid and gaseous impurity, also, obtained synthesis tail gas temperature is 4000 in the synthesis tail gas
~6000K；
(4) first cooling：Synthesis tail gas enters Pen Qing chillings area 104, the area of its runner by synthesis tail gas outlet 103
Increase, flow velocity reduction, be conducive to cooling, also, be that a generation is more complicated anti-because synthesis tail gas exports 103 this segment distance
The process answered, the length of this segment distance is unsuitable oversize, controls in 500mm or so, you can realize that the silane gas reduced after synthesis exists
Decomposed under conditions of high temperature.Synthesis tail gas enters mixes and is cooled to 800 with the normal temperature hydrogen of penetrating behind Pen Qing chillings area 104
Below DEG C, now, the hydrogen content that synthesis tail gas is mixed to form with hydrogen in gaseous mixture, gaseous mixture is increased, and is on the one hand due to
Increase the concentration of hydrogen, reduce the concentration of silane, serve and suppress the effect that silane is decomposed, be on the other hand then effectively to prevent
Only high temperature makes the refrigerant of follow-up hydrojet chilling be decomposed；
(5) cool down again：Gaseous mixture is down into hydrojet chilling area 105, by -10 DEG C~5 DEG C in the hydrojet chilling area
Liquid silicon tetrachloride forms cold atomization area after multigroup sparge pipe and nozzle spray, and gaseous mixture can be cold with atomization after entering
Que Yegai areas complete cold and hot exchange, gaseous mixture is cooled to less than 30 DEG C rapidly；Due to consideration that hydrojet chilling area top
The silicon tetrachloride of penetrating has a possibility being vaporized, and the silicon tetrachloride that this part is vaporized in the cooling procedure of bottom can again by
Liquid is cooled to, therefore, the height in the hydrojet chilling area can design higher, and sparge pipe can design multigroup, to gaseous mixture cooling
It is defined to less than 30 DEG C；
(6) gas-liquid separation：Above-mentioned gaseous mixture and coolant enter gas-liquid separation zone 106 together, and gaseous mixture goes out from synthesis gas
Mouth 9 is discharged, and into silane and hydrogen mixed gas pressure-variable adsorption piece-rate system, and remaining liquid (may carry unreacted silicon
The solid particles such as the silicon that powder, impurity and silane are decomposited) then by entering hydrojet collecting region 107 behind the bottom of gas-liquid separation zone 106,
Due in silane synthetic tower, hydrojet collecting region 107 and solid-liquid mixed collection the area 108 actually region that connects, therefore, solid
Particle is deposited in solid-liquid mixed collection area 108 because of Action of Gravity Field, and liquid then picks out pipe 11 from liquid outlet 14 via liquid
Discharge；Wherein, liquid outlet 14 can also design multigroup, and its every group of connection liquid pick out the caliber of pipe 11 can also design compared with
Greatly, and liquid pick out pipe 11 be designed as it is inverted U-shaped, then be easy for control liquid level, be mixed in the fraction solids particle in liquid
Acted on, can be deposited in the second downward solid-liquid outlet 13 by this U-shaped structure in the end of liquid outlet 14, and from
This enters in silica powder drying device M；And be deposited on the solidliquid mixture in solid-liquid mixed collection area 108 and (include silica flour and other are solid
Body impurity, silicon tetrachloride liquid etc.) regularly entered by the first solid-liquid outlet 12 in silica powder drying device M.
In addition, the technique further comprises the separation for the gaseous mixture discharged from syngas outlet 9, silicon tetrachloride and hydrogen are followed
Ring, and silica flour recovery, because this technique is more ripe, therefore, make simple Jie only in conjunction with the synthesis technique of the present embodiment
Continue.
Specifically, the gaseous mixture discharged from syngas outlet 9 enters silane and hydrogen mixed gas pressure-variable adsorption segregative line
After system, absorption item is silane, and the hydrogen after being handled through pressure-swing absorber L pressure-variable adsorptions enters in pressurization cycle system, and enters
Hydrogen-holder T, then after hydrogen gas compressor T1 superchargings, enter jet chilling system to plasma generator hydrogen supply and after cooling down respectively
System 104；Gaseous silane and hydrogen mixed gas after silane and the processing of hydrogen mixed gas pressure-variable adsorption piece-rate system enter silane
With Hydrogen cryogenic separation and recovery system, gaseous silane is changed into about -112 DEG C of temperature by silane and Hydrogen cryogenic separator S deep coolings
Liquid silane, hydrogen is discharged at the top of silane and hydrogen gas segregator S, into pressurization cycle system, and plasma hair is given respectively
Enter jet chilling system 104 after raw device hydrogen supply and cooling；And silane is then discharged by silane and hydrogen gas segregator S middle part, enter
Enter silane wet tank V, then silane vaporizer W is inputted by silane liquid pump V1, the silane after vaporization is buffered into silane gas
Tank X is temporarily stored, then feeding silane gas storage tank X2 is stored after silane gas compressor X1 pressurizations；In silane and Hydrogen Separation
The liquid of other metallic compound solid residues and silicon tetrachloride will be discharged in device S bottom, and these mixtures will be fed into other gold
The liquid of category compound solid residue and silicon tetrachloride is separated again, and liquid waste treatment system processing is sent into after processing；
The liquid for picking out the discharge of pipe 11 via liquid from liquid outlet 14 enters liquid refrigerants cooling recirculation system, that is, enters
Enter silicon tetrachloride cooling device Q, silicon tetrachloride is stored into silicon tetrachloride storage tank Y after cooling, by silicon tetrachloride liquid pump Y1
Cold night entrance 8 is sent into, and feeding silicon tetrachloride vaporization device P supplies silicon tetrachloride gas to silica powder drying device M；
And silica flour recovery system is then the impurity for making to be discharged into silica powder drying device M, after steam heating, by silicon tetrachloride vapour
Change, the solid after being separated in the equipment is blown afloat (half fluidisation shape) by the gaseous silicon entered by silica powder drying device M bottoms, with
Reach sufficient drying；Gas is discharged into silica flour accurate filter Z by silica powder drying device M top and carries out gas solid separation；Stop
Stay in the timing of the silica flour in silica powder drying device and silica flour collecting box be expelled to by the bottom of silica powder drying device, the silica flour of this part need through
Make the selection of its situation return in silica flour storage tank A after inspection to recycle；
Silicon tetrachloride and silica flour into silica flour accurate filter Z are separated herein, and the tail gas after separation enters four
Silicon chloride cooler R, silicon tetrachloride after cooling enters silicon tetrachloride storage tank Y, enters four chlorinations through silicon tetrachloride liquid pump
Silicon cycling system；Silica flour after separation enters silica flour collecting tank O, and the silica flour of this part need to be such that its situation selects through gas after inspection
Gu conveyer O1 is returned in silica flour storage tank A and recycled；
Silane liquid through discharge in the middle part of silane and hydrogen gas segregator S, into silane wet tank V, then by silane liquid
Pump V1 inputs silane vaporizer W, and the silane after vaporization is temporarily stored into silane gas surge tank X, then is compressed through silane gas
Feeding silane gas storage tank X2 storages after machine X1 pressurizations；At this moment the silane obtained is the first product after fore-running.According to right after after testing
Considered further that the need for silane is different and rectifying again is carried out to it, to reach different grades of silane product.
With discrimination method production silane widely used at present as a comparison, the synthesis technique of the present embodiment silane is carried out
It is further described.
Traditional discrimination method production silane needs to set following device：Liquid chlorine is stored and vapourizing unit；Hydrogen chloride synthesis device；
Trichlorosilane is synthesized and tail gas separation retracting device；Silicon tetrachloride and trichlorosilane topping plant and rectifier unit；Two grades of vaporizations
Produce silane plants；Cold hydrogenation apparatus；Silicon tetrachloride is stored；Trichlorosilane is stored；Silane is stored；
And need to set following device in the production of the present embodiment synthetic method：(because of the consumption very little of silicon tetrachloride, do not disappear substantially
Consumption, using the form of outsourcing) hydrogen Plasma synthesis silane and tail gas and Liquid segregation retracting device；Silane topping plant；Silane
Storage；Silicon tetrachloride is stored；
Advantage as can be seen here using the technology of hydrogen plasma method synthesizing silane is very big, can greatly reduce project construction
Cost and production cost, save project land used, energy consumption is low, environmental protection.
And simulated budget is carried out to difference of the above two technology under the conditions of same size in terms of construction investment, draw：
Investment using hydrogen plasma method synthesizing silane technology than producing silane technology using discrimination method will save 50%, comprehensive energy consumption
Can be low by 50%.And because of the chemical reaction without chlorine in process of production, hydrogen plasma method synthesis silicon in terms of environmental protection is produced
Alkane technology there is no pollution.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention
Enclose, as long as the present invention body design thought and mentally make have no the change of essential meaning or polishing, it is solved
Technical problem it is still consistent with the present invention, should be included in protection scope of the present invention within.
Claims (10)
1. a kind of device of hydrogen plasma method synthesizing silane, it is characterised in that including housing and plasma generator；The housing
Inside it is set to plasma generating region (101), silane synthesis zone (102), Pen Qing chillings area (104), hydrojet chilling successively from top to bottom
Internal diameter is additionally provided between area (105) and gas-liquid separation zone (106), and silane synthesis zone and Pen Qing chillings area from top to bottom gradually to increase
Big synthesis tail gas outlet (103)；The plasma generator negative pole is upward, positive pole is directed downwardly is arranged on plasma generating region
(101) in, the plasma generating region side is provided with raw hydrogen entrance (15)；The silane synthesis zone (102) is provided with sideways
Raw material particulate silicon inlet (4)；The Pen Qing chillings area (104) is uniformly provided with some cold conditions hydrogen entrances (6) sideways；The hydrojet
Chilling area (105) bottom sides are provided with multiple cold liquid entrances (8), and hydrojet chilling area inner homogeneous is provided with multigroup sparge pipe (7), and
Some nozzles are uniformly provided with every group of sparge pipe, the entrance of sparge pipe is connected with cold night entrance；The gas-liquid separation zone (106)
Side top is provided with below syngas outlet (9), gas-liquid separation zone and is set to liquid outlet.
2. a kind of device of hydrogen plasma method synthesizing silane according to claim 1, it is characterised in that the gas-liquid separation
The longitudinal section in area (106) is in convex shape, and the syngas outlet (9) is in inverted L-shaped, and syngas outlet is arranged on gas-liquid separation zone
The top of lateral spine.
3. a kind of device of hydrogen plasma method synthesizing silane according to claim 1 or 2, it is characterised in that the housing
Hydrojet collecting region (107) and solid-liquid mixed collection area (108) are also sequentially provided with below interior gas-liquid separation zone；The hydrojet collecting region
(107) it is in reverse frustoconic structure, hydrojet collecting region side middle and upper part is provided with liquid outlet (14)；The solid-liquid mixed collection area
(108) bottom is provided with the first solid-liquid outlet (12).
4. a kind of device of hydrogen plasma method synthesizing silane according to claim 3, it is characterised in that the liquid discharge
Mouthful (14) are horizontally disposed with, and liquid outlet is provided with the second downward solid-liquid outlet (13), and U is fallen in liquid outlet end provided with one
Shape liquid picks out pipe (11)；The second solid-liquid outlet (13) is higher than hydrojet collecting region (107) bottom, and the liquid connects
Outlet pipe (11) highest point is less than syngas outlet (9) bottom, and liquid is picked out at the top of pipe lowest part hydrojet collecting region (107).
5. a kind of device using described in claim 4 is come the method for synthesizing silane, it is characterised in that by excessive hydrogen and silicon
Powder is passed through in the device of hydrogen plasma method synthesizing silane, and plasma generator ionizes silica flour and excessive hydrogen ionization
Rear hydrogen and the abundant haptoreaction of silicon, obtain the synthesis tail gas being mainly made up of silane and hydrogen, then by the synthesis tail gas first with
Hydrogen mixing chilling, obtains gaseous mixture, then gaseous mixture is mixed into chilling with coolant, finally again by gaseous mixture and coolant point
From, you can obtain including the gaseous mixture of synthesizing silane.
6. the method for utilization hydrogen plasma method synthesizing silane according to claim 5, it is characterised in that including following step
Suddenly：
The A preparatory stages：The gas in the device of hydrogen plasma method synthesizing silane is all first replaced into hydrogen, synthesis gas is then turned on
(9), cold conditions hydrogen entrance (6), cold liquid entrance (8) are exported, is reached to hydrojet collecting region (107) interior liquid level after design liquid level,
Start plasma generator, plasma generating region (101) is produced electric arc；
B plasmas：Raw hydrogen entrance (15) is opened, hydrogen with pressure is heated rapidly by plasma generating region (101)
And after being ionized, into silane synthesis zone (102)；
C is synthesized：Raw material particulate silicon inlet (4) is opened, silica flour is passed through to silane synthesis zone (102) is interior, into the silicon of silane synthesis zone
The high-temperature fusion of the plasma of quilt, vaporization, to plasma, are the hydrogen and silicon synthesizing silane of plasma shape, obtained powder rapidly
Synthesis tail gas, obtained synthesis tail gas temperature is 4000~6000K；
D is cooled down for the first time：Synthesis tail gas exports (103) by synthesis tail gas and enters Pen Qing chillings area (104), sprays into the hydrogen of normal temperature
Mixed with synthesis tail gas, synthesis tail gas is cooled to less than 800 DEG C, also, synthesis tail gas is mixed to form gaseous mixture with hydrogen；
E is cooled down again：Gaseous mixture passes through sparge pipe down into hydrojet chilling area (105) in the hydrojet chilling area by coolant
After being sprayed with nozzle, form cold atomization area, gaseous mixture can be completed after entering with atomized liquid coolant in the area it is cold and hot exchange, make to mix
Close gas and be cooled to less than 30 DEG C；
F gas-liquid separations：Above-mentioned gaseous mixture and coolant enter gas-liquid separation zone (106) together, and gaseous mixture is from syngas outlet (9)
Discharge, and remaining liquid is then discharged by gas-liquid separation zone bottom.
7. the method for utilization hydrogen plasma method synthesizing silane according to claim 6, it is characterised in that the step (6)
In, the remaining liquid enters back into liquid discharge by entering hydrojet collecting region (107) behind gas-liquid separation zone (106) bottom
Mouth (14) picks out pipe (11) discharge via liquid.
8. the method for the utilization hydrogen plasma method synthesizing silane according to claim 6 or 7, it is characterised in that the step
(6) in, after gaseous mixture is handled through pressure-variable adsorption, silane and hydrogen partial are adsorbed, free hydrogen discharge；Hydrogen after discharge enters
Enter hydrogen-holder, then after being pressurized through hydrogen gas compressor, give plasma generator hydrogen supply respectively, and to Pen Qing chillings area after can cooling down
Hydrogen supply；Enter separator after silane after absorption and hydrogen desorption, through deep cooling, gaseous silane is changed into liquid silane, and hydrogen
Gas is then discharged into above-mentioned hydrogen-holder at the top of separator and circulated；Liquid silane is discharged in the middle part of separator, into silicon
Alkane wet tank.
9. the method for utilization hydrogen plasma method synthesizing silane according to claim 8, it is characterised in that the silica flour particle diameter
Less than 0.1mm.
10. the method for the utilization hydrogen plasma method synthesizing silane according to claim 6 or 9, it is characterised in that the cooling
Liquid is liquid silicon tetrachloride, and the silicon tetrachloride temperature is -10 DEG C~5 DEG C.
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| US20100290972A1 (en) * | 2006-10-02 | 2010-11-18 | Solaria Tecnologie S.R.L. | Process and device for the production of high-purity silicon using multiple precursors |
| CN207294192U (en) * | 2017-08-31 | 2018-05-01 | 许文 | A kind of hydrogen plasma method silane synthetic tower |
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| US20040091412A1 (en) * | 2000-04-07 | 2004-05-13 | Dirk Muller | Method and facility for producing silane |
| US20100290972A1 (en) * | 2006-10-02 | 2010-11-18 | Solaria Tecnologie S.R.L. | Process and device for the production of high-purity silicon using multiple precursors |
| CN101541814A (en) * | 2006-12-01 | 2009-09-23 | 罗斯顿家族有限责任公司 | Process for preparation of alkoxysilanes |
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