CN106672979A - Device and method for continuously preparing silicane and disilane through magnesium silicide method - Google Patents
Device and method for continuously preparing silicane and disilane through magnesium silicide method Download PDFInfo
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- CN106672979A CN106672979A CN201510753956.3A CN201510753956A CN106672979A CN 106672979 A CN106672979 A CN 106672979A CN 201510753956 A CN201510753956 A CN 201510753956A CN 106672979 A CN106672979 A CN 106672979A
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- Prior art keywords
- reactor
- filter
- outlet
- liquefied ammonia
- drier
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 57
- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 55
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 246
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 99
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 229910021529 ammonia Inorganic materials 0.000 claims description 118
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical group [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 84
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 42
- 239000000126 substance Substances 0.000 claims description 34
- 229910007981 Si-Mg Inorganic materials 0.000 claims description 31
- 229910008316 Si—Mg Inorganic materials 0.000 claims description 31
- 229910045601 alloy Inorganic materials 0.000 claims description 31
- 239000000956 alloy Substances 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 29
- 239000007788 liquid Substances 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 19
- 229910000077 silane Inorganic materials 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 239000012265 solid product Substances 0.000 claims description 12
- 239000000460 chlorine Substances 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 8
- 239000010802 sludge Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 239000012429 reaction media Substances 0.000 abstract description 5
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000861 Mg alloy Inorganic materials 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 41
- 229910052710 silicon Inorganic materials 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 239000000843 powder Substances 0.000 description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 9
- 229910052749 magnesium Inorganic materials 0.000 description 9
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 238000003860 storage Methods 0.000 description 9
- -1 silicon Alkane Chemical class 0.000 description 7
- 238000005660 chlorination reaction Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910019752 Mg2Si Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006073 displacement reaction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000008247 solid mixture Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229910003641 H2SiO3 Inorganic materials 0.000 description 1
- VCOYRKXQRUGBKS-UHFFFAOYSA-N N.[Cl] Chemical compound N.[Cl] VCOYRKXQRUGBKS-UHFFFAOYSA-N 0.000 description 1
- 229910007264 Si2H6 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007805 chemical reaction reactant Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000029142 excretion Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012065 filter cake Substances 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
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000004826 seaming Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for continuously preparing silicane and disilane through a magnesium silicide method. According to the method, flowing liquid ammonia is utilized as a reaction medium, magnesium silicide or silicon-magnesium alloy and ammonium chloride finish reaction in medium flow. The invention further discloses a device for continuously preparing the silicane and the disilane through the magnesium silicide method. The method and the device can achieve the purpose of generating the silicane and the disilane gas stably, continuously and safely.
Description
Technical field
The present invention relates to magnesium silicide method prepares monosilane and disilane technique.More particularly, to a kind of silicon
Change the apparatus and method that magnesium processes continuously prepare monosilane and disilane.
Background technology
Traditionally, the technique that magnesium silicide method prepares silane is all step, and this is because development one is continuous
There are many difficulties in the magnesium silicide method technique of operation.
On the one hand, there is gas, liquid, solid three-phase simultaneously in the reaction.Gas phase includes that product silane mixture is (main
To include monosilane and disilane) and byproduct hydrogen gas, this several person can occur when air is run into spontaneous combustion from
It is quick-fried.Liquid phase is reaction medium liquefied ammonia, and its saturated vapour pressure is high, excitant is strong, strong toxicity, while also having
The danger of blast.When the presence of this air-liquid two-phase causes to prepare monosilane and disilane using the reaction,
Sealing property requirement to the equipment of reaction system is very high.And the magnesium silicide or Si-Mg alloy in the reaction
Reactant and magnesium chloride hexammoniates such as (silicon-magnesium alloy, United States Patent (USP)s US4808392)
All it is solid phase Deng accessory substance, this solid material and product can carry out generation resistance to reaction, therefore should
Reaction will have good solid-liquid mass transfer.More importantly, in order to realize the reuse to liquefied ammonia and to six ammonia chlorine
The thermal decomposition for changing magnesium is reclaimed, and needs to separate in the accessory substances such as magnesium chloride hexammoniate and reaction medium liquefied ammonia, and this is just needed
Want reaction system that there is reliable liquid-solid separation device.
Chinese patent CN101798085A has done a good try, and this application adopts plural serial stage autoclave
Silane reactor preparing silane, by the way that the control of every stage reactor is improved into silane in different reaction temperatures
Gas production.But because this application needs to combine multiple tank reactors, using multigroup condenser, scrubbing tower,
Pump etc. is produced with suspension, operation is complicated, realizes that difficulty is big.Material from leakage, gas-liquid between simultaneous reactions device
Two-phase has that caused security of system is still present, and does not consider separation of solid and liquid problem.
The recoverying and utilizing method of Chinese patent CN101928013A ammonia in slurry of silane generator, by by silicon
Alkane generator slurry be placed on can by wabbler mechanism in the Filter dryer for longitudinally rotate certain angle come
Control the motion of suspension and filter cake to realize filtering the switching with dry run.But, for a pressure
Container and its connecting pipe, if continually rotating it, then the sealing property of the device certainly will be required very
It is good, the leakage of the silane to prevent liquefied ammonia and be dissolved in liquefied ammonia.Even if sealing property reaches requirement, repeatedly
After rotation, unavoidably occur that sealing property declines, this will bring hidden to the safety problem of staff
Suffer from.
Therefore, also it is not carried out No leakage, can continuously producing silicon under an increased pressure in prior art
Alkane, and continuously by magnesium chloride hexammoniate and Ammonia separation and by the device and technique of liquefied ammonia recycling use.
The content of the invention
It is an object of the present invention to provide a kind of magnesium silicide method continuously prepares the side of monosilane and disilane
Method.
Further object is that providing a kind of magnesium silicide method continuously prepares monosilane and disilane
Device.
Magnesium silicide method prepares the fundamental reaction formula of silane：
Mg2Si+4NH4Cl+8NH3=2Mg (NH3)6Cl2+SiH4
2Mg2Si+8NH4Cl+16NH3=4Mg (NH3)6Cl2+Si2H6+H2
It is appreciated that when using Si-Mg alloy, reacting the accessory substance for generating and also having in addition to magnesium chloride hexammoniate
Other chloride by-products.
The present invention adopts following technical proposals：
A kind of method that magnesium silicide method continuously prepares monosilane and disilane, comprises the following steps：
Liquefied ammonia is squeezed into reactor from wet tank with circulating pump；
By the mixture of magnesium silicide or Si-Mg alloy and ammonium chloride it is continuous, be homogeneously added into reactor；
Mixture starts reaction after contacting with liquefied ammonia, generate monosilane and disilane mixture and six ammonia chlorinations
The accessory substances such as magnesium；
Monosilane and disilane mixture discharge reactor, are received by gas reception device, obtain thick first silicon
Alkane and b silane gas；
After the accessory substances such as the magnesium chloride hexammoniate of generation are with liquefied ammonia outflow reactor, using filter by liquefied ammonia with
The accessory substances such as magnesium chloride hexammoniate are separated, and liquefied ammonia returns to after cooling wet tank.
A kind of method that magnesium silicide method continuously prepares monosilane and disilane, comprises the following steps：
The mixed liquor of liquefied ammonia and ammonium chloride is squeezed into reactor from wet tank with circulating pump；
By magnesium silicide or Si-Mg alloy it is continuous, be homogeneously added into reactor；
Magnesium silicide or Si-Mg alloy start reaction after contacting with mixed liquor, generate monosilane and disilane mixing
The accessory substance such as thing and magnesium chloride hexammoniate；
Monosilane and disilane mixture discharge reactor, are received by gas reception device, obtain thick first silicon
Alkane and b silane gas；
After the accessory substances such as the magnesium chloride hexammoniate of generation are with liquefied ammonia outflow reactor, using filter by liquefied ammonia with
The accessory substances such as magnesium chloride hexammoniate are separated, and liquefied ammonia mixes after cooling with ammonium chloride, are formed and are returned to after mixed liquor
Wet tank.
Addition magnesium silicide or Si-Mg alloy powder can be eliminated by the way of prefabricated ammonium chloride liquefied ammonia mixed liquor
The putty phenomenon being likely to occur when end and ammonium chloride mixt.
" Si-Mg alloy " in the present invention, refer to those in order to increase disilane yield and synthesize include non-magnesium
Si-Mg alloy in the Si-Mg alloy of non-element silicon, such as United States Patent (USP) US4808392.Because silicon magnesium is closed
The synthetic method of gold is identical with the synthetic method of magnesium silicide, and form is also all micro-solid powder, therefore at this
The using method of Si-Mg alloy is also identical with the using method of magnesium silicide in invention.
The present invention using circulating pump control liquefied ammonia by with the liquefied ammonia that flow as reaction medium, being flowed so that
Magnesium silicide or Si-Mg alloy and ammonium chloride complete reaction in medium flow field so that the reaction has good consolidating
Liquid mass transfer；The gaseous product of generation is received by gas reception device, and security of system is high；Using filter
Continuously by the accessory substances such as magnesium chloride hexammoniate and Ammonia separation, the continuous operation of magnesium silicide method is realized.Meanwhile,
Several equipment due to only needing fixation, equipment investment is few, simple to operate.
Further, when raw material is magnesium silicide, the accessory substance is magnesium chloride hexammoniate, and methods described is also
Including：Ammonia will be resolved into the accessory substance magnesium chloride hexammoniate after Ammonia separation, ammonia condensation forms liquefied ammonia,
Wet tank is returned to after cooling or is mixed with ammonium chloride, to be formed and return to wet tank after mixed liquor.Separate
The water capacity of magnesium chloride hexammoniate afterwards is generally less than 50%.Preferably, employing can realize from room temperature to
The drier of 300-450 DEG C of thermograde processes magnesium chloride hexammoniate.It is highly preferred that the drier is spiral shell
Rotation blade tube drier, including：Housing, axle, blade；The axle is arranged in housing；The oar
Leaf is arranged on axle；The propeller blade tube drier has feed(raw material)inlet, product gas outlet and consolidates
Body product exit；Top to the end of the propeller blade tube drier has from room temperature to 300-450 DEG C
Thermograde；The product gas outlet, feed(raw material)inlet are arranged adjacent to the top of the drier, institute
The end for stating the neighbouring drier of solid product outlet is arranged.Now, magnesium chloride solids material and ammonia
Do convective motion.Magnesium chloride solids material is descending to high-temperature region, and the free ammonia of absorption volatilizees first, Ran Houpei
Ammonia of the position on magnesium chloride hexammoniate progressively decomposes in drier.And ammonia is up to low-temperature space, high-temperature
Ammonia heats solid material, can so greatly save the thermal energy consumption of drier.In described drier
Gas pressure (- 0.1) -2MPa (gauge pressure, similarly hereinafter), preferably (- 0.1) -1.6MPa.
Further, the gas reception device includes backflow column scrubber and the first condenser；The first silicon
Alkane and disilane mixture discharge reactor, Jing backflow column scrubber washings and the cooling of the first condenser, silane
Most ammonia in mixture is removed, and obtains thick monosilane and b silane gas.Low chilling temperature
Ammonia can be caused, and as far as possible obtaining condensation returns to reactor, but disilane can be caused to liquefy if temperature is too low
(condensing temperature under normal pressure is -14.5 DEG C) and stay in reactor.
Preferably, the time of staying of the reaction mass in liquefied ammonia is 0.1-10h；More preferably 0.1-3h.Stop
The time is stayed to refer to the time of staying of the solid mixture of magnesium silicide or Si-Mg alloy powder and ammonium chloride in liquefied ammonia
Or the time of staying of magnesium silicide or Si-Mg alloy powder in the mixed liquor of liquefied ammonia and ammonium chloride, that is, react
The time of contact of material (magnesium silicide or Si-Mg alloy and ammonium chloride) is 0.1-10h；More preferably 0.1-3h.
Preferably, the concentration of ammonium chloride is 1-30%, preferably 5-25%.
Preferably, the purity of the liquefied ammonia is higher than 99.9%；More preferably purity is higher than 99.999%.Using height
The liquefied ammonia of purity is to ensure the yield of silane.Liquefied ammonia is used as reaction medium, wherein most harmful impurity
Mainly water.Because the presence of water can cause to react produces useless hydrogen, rather than silane.
Producing one possible mechanism of hydrogen is：
Mg2Si+4NH4Cl+8NH3+3H2O=2Mg (NH3)6Cl2+H2SiO3+4H2↑,
Therefore, the presence of water can reduce the yield of silane.
Qi Hongxiang, Wang Kang, chemical industry and engineering technology, 2013,34 (2), 37-40 reports generation hydrogen
Another possible mechanism：
NH4Cl+H2O=HCl+NH3·H2O,
Mg2Si+4HCl+8NH3=2Mg (NH3)6Cl2+Si+2H2↑,
NH3·H2O=NH3+H2O,
According to this principle, the harm of the presence of water is just bigger.
Preferably, the pressure in the reactor is 0-2MPa, preferably 0.8-1.6MPa；The liquid
Pressure in storage tank is 0-0.8MPa.
Preferably, the temperature in the wet tank is (- 30)-(- 10) DEG C.This temperature is than existing
Technology temperature improves, and can greatly reduce the requirement to refrigeration machine, and the raising of reaction temperature is favourable
In the synthesis of disilane.
Further, the temperature control in the reactor is between -50 DEG C of (- 40).In the reactor
Reaction may be at isothermal temperature condition or the alternating temperature temperature conditionss for gradually heating up.Preferably, reactor
Interior reaction is under alternating temperature temperature conditionss.Alternating temperature temperature conditionss are preferably：Material is advanced along in reactor
Direction heat up, and for gradient increased temperature.It is highly preferred that the direction advanced along material in reactor, reaction
Device temperature raises 30-60 DEG C.Most preferably, reactor top temperature is (- 30)-(- 10) DEG C, is reacted
Device terminal temperature is 20-40 DEG C.Compared to isothermal temperature condition, alternating temperature temperature conditionss have the following advantages：Instead
Answer device top corresponding to the new magnesium silicide for adding or the ammonium chloride of Si-Mg alloy powder and high concentration, relatively low rises
Beginning temperature causes reaction to be unlikely to excessively violent；And in reactor end, higher reaction temperature correspond to compared with
Low reactant concentration, can cause reaction to carry out more complete so that the yield of monosilane and disilane is protected
Hold more than 90%；Meanwhile, the presence of thermograde causes reaction speed to accelerate on the whole, improves list
The yield of position equipment.
Because the reaction that magnesium silicide method prepares silane is an exothermic reaction, in the pressure condition that the present invention is selected
Under, the liquefied ammonia in reactor is not vaporized substantially, the temperature of liquefied ammonia with the carrying out of reaction in reactor along
The direction that material is advanced progressively raises naturally.It is different with the rate of charge of magnesium silicide or Si-Mg alloy according to liquefied ammonia,
The intensification degree of liquefied ammonia suspension is different.It was found that, feeding intake when liquefied ammonia and magnesium silicide or Si-Mg alloy
During than higher than 15, the thermograde that the reaction carried out in reactor is voluntarily produced is less than normal, at this moment can be using anti-
The outer concurrent heating of device is answered to realize thermograde.
Preferably, the weight ratio of ammonium chloride and magnesium silicide or Si-Mg alloy is 2.8-6 in reactor：1.Chlorination
Ammonium and magnesium silicide theory rate of charge are 2.8, it is done so that may be such that reaction is incomplete, reaction speed
It is partially slow, so control ammonium chloride is suitably excessive.Excessive chloride leach in liquefied ammonia, big portion therein
Branch is circulated with liquefied ammonia, realizes recycling；Can adsorb on a small quantity on accessory substance filter residue, the chlorination of absorption
Ammonium decomposes vaporization under this high-temperature：NH4Cl=NH3+ HCl, with ammonia after cooling, becomes chlorination again
Ammonium：NH3+ HCl=NH4Cl, chloride leach is recycled in liquefied ammonia into ammonia tank.Concrete
During enforcement, generally suitably add ammonium chloride in initial period, 2.8 ratio is remained close to after system stability
Charging.
The present invention also provides a kind of device for being applicable to said method：
A kind of magnesium silicide method continuously prepares the device of monosilane and disilane, including：
Wet tank, circulating pump, reactor, filter, cooler, solid feed pot and gas are received
Device；
Reactor has the outlet of liquid inlet, solid inlet, gas vent and suspension；
Filter has suspension inlet, liquid outlet and sludge outlet；
The outlet Jing circulating pumps of wet tank are connected with the liquid inlet of reactor；
Solid feed pot is connected with the solid inlet of reactor；
The gas vent of reactor is connected with gas reception device；
The suspension outlet of reactor is connected with the suspension inlet of filter；
The liquid outlet of filter is connected with the entrance of cooler；
The outlet of cooler is connected with the entrance of wet tank.
Further, the gas reception device includes backflow column scrubber and the first condenser；Backflow washing
The entrance of post is connected with the gas vent of reactor, and outlet is connected with the first condenser.
Further, described device also includes drier and the second condenser；
Drier has the outlet of feed(raw material)inlet, product gas outlet and solid product；
The feed(raw material)inlet of drier is connected with the sludge outlet of filter, and product gas outlet and second is condensed
The entrance of device is connected；
The outlet of the second condenser is connected with the entrance of wet tank.
Preferably, the drier is propeller blade tube drier, may be simply referred to as tube drier, spiral shell
Rotation blade dryer or blade dryer, including housing, the axle being arranged in housing, be arranged on axle
Blade, with the outlet of feed(raw material)inlet, product gas outlet and solid product.The side of axle is provided with magnetic force drive
Dynamic device, axle Jing magnetic driving equipments drive.Top to the end tool of the propeller blade tube drier
The thermograde having from room temperature to 300-450 DEG C.The product gas outlet, feed(raw material)inlet set adjacent to top
Put, the solid product outlet adjacent end is arranged.The propeller blade tube drier is in hull outside
It is provided with heater.Because making, temperature control or during using needing, propeller blade tube drier is divided into two
Section or multi-stage series composition, each section of diameter and material may be the same or different, and drier segmentation does not change
The foundation of temperature gradient.
Preferably, the solid product outlet of the drier is connected with magnesium chloride storage tank.
Preferably, described device also includes filter residue tank；The sludge outlet phase of the entrance of filter residue tank and filter
Even, outlet is connected with the feed(raw material)inlet of drier.
Further, described device also includes：Ammonium chloride liquefied ammonia prefabricated tanks；The outlet of the second condenser
It is connected with the entrance of ammonium chloride liquefied ammonia prefabricated tanks, the outlet of ammonium chloride liquefied ammonia prefabricated tanks and entering for wet tank
Mouth is connected.
Further, described device also includes self-conveyor feed；Solid feed pot Jing self-conveyor feeds with it is anti-
The solid inlet for answering device is connected.Self-conveyor feed can ensure that magnesium silicide or Si-Mg alloy powder or
Mixture with ammonium chloride is continuous for it, be homogeneously added into reactor.
Further, the reactor is tubular reactor, preferably horizontal tube, vertical pipe type, coil pipe
Formula or U-shaped tubular reactor.Further, the reactor be without stirring tubular reactor or
Tubular reactor with stirring.Preferably, because making or using needing, tubular reactor being divided into two sections
Or multi-stage series composition, each section of diameter, structure and agitating mode may be the same or different, reactor
Segmentation does not change the selection of temperature parameter.
Preferably, the pressure in the reactor is 0-2MPa, preferably 0.8-1.6MPa；The liquid
Pressure in storage tank is 0-0.8MPa.
Preferably, the temperature in the wet tank is (- 30)-(- 10) DEG C.Pressure in wet tank
Power is corresponding with the pressure of the gas vent of filter.Pressure is at the suspension inlet of filter
0.8-1.6MPa, gas outlet pressure is 0-0.8MPa.
Further, the reactor outside is provided with external heat exchanger.External heat exchanger is provided with heat transferring medium and enters
Mouth and heat transferring medium outlet, heat transferring medium entrance is positioned close to the side of the outlet of reactor, and heat exchange is situated between
Matter outlet is positioned close to the side of the entrance of reactor.
Further, the reactor is provided with least one radial agitator, including the first shaft and
The radial direction stirring vane being arranged on the first shaft.When several radial agitators are provided with, with each
Radial agitator is boundary, and the external heat exchanger is made up of several sections, and there is each section respective heat exchange to be situated between
Matter entrance and heat transferring medium are exported.
Further, axial agitator is provided with the reactor, including the second shaft and is arranged on the
Axial stirring vane on two shafts.
Further, the filter is using the pressure reduction between reactor and wet tank as filtration power.
Preferably, the filter is continuous filter, to realize continuous solid-liquor separation.It is more preferably continuous
Pressing filter or screw extrusion filter.Most preferably, the continuous pressing filter is pressurization rotation
Filter；Particularly Barrate type filter, rotary drum type filter or collar plate shape filter.The filter
In filter medium be preferably 10-1000 mesh stainless (steel) wires.When reactor is the tubular type with axial agitator
Reactor, and the filter for pressurization rotary filter when, the stirring of tubular reactor and filter
Rotation can adopt same magnetically-actuated source.The rotating speed phase that the rotating speed and filter of reactor stirring is rotated
It is same or different.If both rotating speeds are different, by adding speed changer both rotating speeds can be made consistent.Instead
The combination for answering device and filter is installed to enable to complete to react the suspension for obtaining and directly filtered, fully
The pressure carried using material.
Further, in described device, power is magnetically-actuated.
Beneficial effects of the present invention are as follows：
1st, the inventive method constructs the medium of the liquefied ammonia circulation as reaction of a flowing, magnesium silicide or silicon
Magnesium alloy and ammonium chloride complete reaction in medium flow field, can stablize, continuously produce monosilane and second silicon
Alkane gas, the accessory substance separating and recovering such as liquefied ammonia and magnesium chloride hexammoniate after the completion of reaction is realized real continuous
Magnesium silicide method prepare monosilane and disilane technique.
2nd, device of the invention is closed-loop technique, and without environmental pollution, system is safer, improves silicon
The quality of alkane.
Description of the drawings
The specific embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 is the schematic device of the present invention；
Fig. 2 is the tubular reactor schematic diagram without stirring；
Fig. 3 is the tubular reactor schematic diagram with radial direction stirring；
Fig. 4 is the tubular reactor schematic diagram with axially stirring；
Fig. 5 is to be raised by the thermogenetic temperature of reaction and the graph of a relation between liquefied ammonia and magnesium silicide charge ratio；
Fig. 6 is the optimizing technology parameters of the present invention；
Fig. 7 is the schematic diagram of the propeller blade tube drier with blade.
Specific embodiment
In order to be illustrated more clearly that the present invention, the present invention is done into one with reference to preferred embodiments and drawings
The explanation of step.Similar part is indicated with identical reference in accompanying drawing.Those skilled in the art
It should be appreciated that following specifically described content is illustrative and be not restrictive, should not be limited with this
Protection scope of the present invention.
As shown in figure 1, the magnesium silicide method for the present invention continuously prepares the device 200 of monosilane and disilane,
Including：
Wet tank 210, circulating pump 220, reactor 230, filter 240, cooler 250, solid
Feed pot 260, self-conveyor feed 262, gas reception device 273 are (including backflow column scrubber 270 and the
One condenser 272), filter residue tank 280, the condenser 284 of propeller blade tube drier 282 and second；
Reactor 230 has the outlet of liquid inlet, solid inlet, gas vent and suspension；
Filter 240 has suspension inlet, liquid outlet and sludge outlet；
The outlet Jing circulating pumps 220 of wet tank 210 are connected with the liquid inlet of reactor 230；
The Jing self-conveyor feeds 262 of solid feed pot 260 are connected with the solid inlet of reactor 230；
The entrance of backflow column scrubber 270 is connected with the gas vent of reactor 230, and outlet is condensed with first
Device 272 is connected；The outlet of the first condenser 272 is provided with pressure valve 274, for controlling the first condenser
272 pressure；
The suspension outlet of reactor 230 is connected with the suspension inlet of filter 240；
The liquid outlet of filter 240 is connected with the entrance of cooler 250；
The outlet of cooler 250 is connected with the entrance of wet tank 210；
Drier 282 has feed(raw material)inlet 2822, product gas outlet 2823 and solid product outlet 2824,
The entrance of filter residue tank 280 is connected with the sludge outlet of filter 240, the raw material of outlet and drier 282
Entrance is connected, and the product gas outlet of drier 282 is connected with the entrance of the second condenser 284；Second
The outlet of condenser 284 is connected with the entrance of wet tank 210.The solid product outlet of drier 282
It is connected with magnesium chloride storage tank 286.
In another embodiment, described device also includes：Ammonium chloride liquefied ammonia prefabricated tanks 212；Second is cold
The outlet of condenser 284 is connected with the entrance of ammonium chloride liquefied ammonia prefabricated tanks 212, ammonium chloride liquefied ammonia prefabricated tanks 212
Outlet be connected with the entrance of wet tank 210.
The reactor 230 is tubular reactor, preferably horizontal tube, vertical pipe type, coiled or U
Type tubular reactor.Pressure in reactor 230 is 0-2MPa, preferably 0.8-1.6MPa；Liquid is stored up
Pressure in tank 210 is 0-0.8MPa.Temperature in wet tank 210 is (- 30)-(- 10) DEG C.
Pressure in wet tank 210 is corresponding with the pressure of the gas vent of filter 240.Filter it is outstanding
Supernatant liquid pressure at inlet is 0.8-1.6MPa, and gas outlet pressure is 0-0.8MPa.
As shown in Fig. 2 the outside of reactor 230 is provided with external heat exchanger 231.External heat exchanger 231 is provided with and changes
Thermal medium entrance 232 and heat transferring medium outlet 233, heat transferring medium entrance 232 is positioned close to reactor
The side of 230 outlet, heat transferring medium outlet 233 is positioned close to the side of the entrance of reactor 230.
290 represent liquefied ammonia or liquefied ammonia and ammonium chloride mixed liquor.292 represent magnesium silicides or Si-Mg alloy powder or
Person its mixture with ammonium chloride.294 represent the accessory substance such as liquefied ammonia and magnesium chloride hexammoniate and unreacted chlorine
Change the suspension of ammonium.
As shown in figure 3, reactor 230 is provided with least one radial agitator 235, including the first stirring
Axle 234 and the radial direction stirring vane 236 being arranged on the first shaft 234.Radially stir when several are provided with
When mixing device 235 (235 ', 235 "), and each agitator 235 (235 ', 235 ") stir including first respectively
The radial direction mixed axle 234 (234 ', 234 ") and be arranged on the first shaft 234 (234 ', 234 ") is stirred
Mix blade 236 (236 ', 236 ").With each radial agitator as boundary, the external heat exchanger is by several
Section heat exchanger 231 (231 ', 231 ", 231 " ') composition, there is each section respective heat transferring medium to enter
Mouthfuls 232 (232 ', 232 ", 232 " ') and heat transferring medium export 233 (233 ', 233 ", 233 " ').
As shown in figure 4, being provided with axial agitator 237, including the second shaft in the reactor 230
238 and the axial stirring vane 239 that is arranged on the second shaft 238.
Radial agitator 235 and axial agitator 237 are magnetically-actuated.
The filter 240 using the pressure reduction between reactor 230 and wet tank 210 as filter power,
Filter 240 is preferably magnetically-actuated.Preferably, the filter 240 is continuous filter, with reality
Existing continuous solid-liquor separation.More preferably continuous pressing filter or screw extrusion filter.Most preferably,
The continuous pressing filter is pressurization rotary filter；Particularly Barrate type filter, rotary drum type are filtered
Machine or collar plate shape filter.Filter medium in the filter 240 is preferably 10-1000 mesh stainless steels
Net.When reactor 230 is the tubular reactor with axial agitator 237, and the filter 240
For pressurize rotary filter when, the stirring of tubular reactor 230 and the rotation of filter 240 can be adopted
Same magnetically-actuated source.Reactor 230 stirring rotating speed it is identical with the rotating speed that filter 240 is rotated or
It is different.If both rotating speeds are different, by adding speed changer both rotating speeds can be made consistent.Reactor 230
Install to enable to complete to react the suspension for obtaining with the combination of filter 240 and directly filter, fully
The pressure carried using material.
As shown in fig. 7, be the structural representation of propeller blade tube drier 282, including housing 2821,
The axle 288 being arranged in housing, the blade 289 being arranged on axle 288.The side of axle 288 is provided with magnetic force
Driving means 287, axle Jing magnetic driving equipments drive.The top of the propeller blade tube drier 282
There is the thermograde from room temperature to 300-450 DEG C to end.The product gas outlet 2823, raw material enters
Mouth 2822 is arranged adjacent to top, and the solid product exports 2824 adjacent ends and arranges.The screw
Blade tube type drier 282 is provided with heater 283 in hull outside, so as to realize from room temperature to
300-450 DEG C of thermograde.296 represent magnesium chloride hexammoniate filter residue.297 represent ammonia.298 represent chlorine
Change magnesium.
Wet tank 210 is used for depositing the liquefied ammonia or the second condenser 284 of the outflow of cooler 250 and flows
Ammonium chloride and the mixture of liquefied ammonia that the liquefied ammonia for going out or ammonium chloride liquefied ammonia prefabricated tanks 212 flow out.Liquid
The opposite side of the outlet of storage tank 210 is provided with ammonia excretion valve 214.
Circulating pump 220 is used for for liquid squeezing into the high reactor 230 of pressure from the low wet tank 210 of pressure
It is interior.Circulating pump 220 can select any 0.8MPa that can produce with the pump of seaming chuck.Preferably, it is described
Circulating pump be positive displacement circulating pump, more preferably magnetically-actuated vane pump (being also called sliding-vane pump, ammonia pump),
Membrane pump.Magnetically-actuated can be completely isolated with air by reaction unit, realizes the zero leakage of gas phase and liquid phase.
During using the device of the present invention continuously to prepare monosilane and disilane, there are two kinds of implementations.
Embodiment 1
Liquid in wet tank 210 is liquefied ammonia, is comprised the following steps：
1) to whole device first with nitrogen displacement three times, then replaced three times with ammonia.
2) liquefied ammonia is squeezed into tubular reactor 230 from wet tank 210 by circulating pump 220, liquid
The direction flow forward that ammonia is advanced along material in reactor 230, through filter 240 and cooler 250,
Wet tank 210 is eventually passed back to, to set up a liquefied ammonia circulation.The purity of liquefied ammonia is higher than 99.9%；It is more excellent
Purity is selected to be higher than 99.999%.
3) solid mixture of magnesium silicide or Si-Mg alloy and ammonium chloride is entered into spiral shell by solid feed pot 260
(the rate of charge 2.8-6 of ammonium chloride and magnesium silicide or Si-Mg alloy in rotation charger 262：, and Jing spirals 1)
Charger 262 enters reactor 230.
4) in the presence of liquefied ammonia, magnesium silicide or Si-Mg alloy and ammonium chloride start reaction, in reactor 230
The middle generation accessory substance such as monosilane and disilane mixture and magnesium chloride hexammoniate.Reaction mass is in liquefied ammonia
The time of staying is 0.1-10h；More preferably 0.1-3h.Reactor top temperature is (- 30)-(- 10) DEG C,
Reactor terminal temperature is 20-40 DEG C.Pressure in reactor is 0.8-1.6MPa；In the wet tank
Pressure be 0-0.8MPa, temperature be (- 30)-(- 10) DEG C.Monosilane and disilane mixture are gas
Phase, the gas vent of reacted device 230 enters backflow column scrubber 270 and washs, and the first condensers of Jing 272
Cooling, obtains thick monosilane and b silane gas.It is the accessory substances such as the magnesium chloride hexammoniate of generation, unreacted
Ammonium chloride enters filter 240 with the suspension outlet of the reacted device 230 of suspension that liquefied ammonia is formed together.
5) process through filter 240, the accessory substance such as liquefied ammonia and magnesium chloride hexammoniate is separated, liquefied ammonia and unreacted
Ammonium chloride Jing cooler 250 cooling after enter wet tank 210 in.The accessory substances such as magnesium chloride hexammoniate enter
In entering filter residue tank 280.When raw material is magnesium silicide, only have magnesium chloride hexammoniate, six ammonia chlorinations in accessory substance
Enter in propeller blade tube drier 282 after magnesium, magnesium chloride and ammonia, ammonia are resolved into wherein
Into in the second condenser 284, it is condensed into after liquefied ammonia and enters wet tank 210.Magnesium chloride enters magnesium chloride
In storage tank 286.
Jing is tested, and the gross production rate of monosilane and disilane is more than 90%.According in synthesis Si-Mg alloy powder
The species of the non-magnesium non-silicon metals added when last and the difference of amount, the yield of disilane is in 1-40% scopes
It is interior.
Embodiment 2
Liquid in wet tank 210 is the mixed liquor of liquefied ammonia and ammonium chloride, is comprised the following steps：
1) to whole device first with nitrogen displacement three times, then replaced three times with ammonia.
2) liquefied ammonia and ammonium chloride mix first in ammonium chloride liquefied ammonia prefabricated tanks 212, by circulating pump 220
Mixed liquor is squeezed into tubular reactor 230 from wet tank 210, mixed liquor is along reactor 230
The direction flow forward that middle material is advanced, through filter 240 and cooler 250, eventually passes back to liquid storage
Tank 10, to set up a liquefied ammonia circulation.The purity of liquefied ammonia is higher than 99.9%；More preferably purity is higher than
99.999%.
3) magnesium silicide or Si-Mg alloy powder enter (chlorine in self-conveyor feed 262 from solid feed pot 260
Change the rate of charge 2.8-6 of ammonium and magnesium silicide or Si-Mg alloy：1), and Jing self-conveyor feeds 262 enter reaction
Device 230.
4) in the presence of liquefied ammonia, magnesium silicide or Si-Mg alloy and ammonium chloride start reaction, in reactor 230
The middle generation accessory substance such as monosilane and disilane mixture and magnesium chloride hexammoniate.Reaction mass is in liquefied ammonia
The time of staying is 0.1-10h；More preferably 0.1-3h.Reactor top temperature is (- 30)-(- 10) DEG C,
Reactor terminal temperature is 20-40 DEG C.Pressure in reactor is 0.8-1.6MPa；In the wet tank
Pressure be 0-0.8MPa, temperature be (- 30)-(- 10) DEG C.Monosilane and disilane mixture are gas
Phase, the gas vent of reacted device 230 enters backflow column scrubber 270 and washs, and the first condensers of Jing 272
Cooling, obtains thick monosilane and b silane gas.It is the accessory substances such as the magnesium chloride hexammoniate of generation, unreacted
Ammonium chloride enters filter 240 with the suspension outlet of the reacted device 230 of suspension that liquefied ammonia is formed together.
5) process through filter 240, the accessory substance such as liquefied ammonia and magnesium chloride hexammoniate is separated, liquefied ammonia and unreacted
Ammonium chloride Jing cooler 250 cooling after enter wet tank 210 in.The accessory substances such as magnesium chloride hexammoniate enter
In entering filter residue tank 280.When raw material is magnesium silicide, only have magnesium chloride hexammoniate, six ammonia chlorinations in accessory substance
Enter in propeller blade tube drier 282 after magnesium.Magnesium chloride hexammoniate resolve into wherein magnesium chloride and
Ammonia, ammonia is entered in the second condenser 284, is condensed into after liquefied ammonia and is entered ammonium chloride solution ammonia prefabricated tanks 212.
Magnesium chloride is entered in magnesium chloride storage tank 286.It is appreciated that in this kind of mode, also including and ammonium chloride solution
The connected ammonium chloride storage tank of ammonia prefabricated tanks 212.
Jing is tested, and the gross production rate of monosilane and disilane is more than 90%.According in synthesis Si-Mg alloy powder
The species of the non-magnesium non-silicon metals added when last and the difference of amount, the yield of disilane is in 1-40% scopes
It is interior.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and
It is not the restriction to embodiments of the present invention, for those of ordinary skill in the field,
Can also make other changes in different forms on the basis of described above, here cannot be to all
Embodiment be exhaustive, it is every to belong to the obvious change that technical scheme is extended out
Change or change the row still in protection scope of the present invention.
Claims (23)
1. a kind of method that magnesium silicide method continuously prepares monosilane and disilane, it is characterised in that include with
Lower step：
Liquefied ammonia is continuously squeezed into reactor from wet tank；
The mixture of magnesium silicide or Si-Mg alloy and ammonium chloride is added continuously in reactor；
Mixture starts reaction after contacting with liquefied ammonia, generate monosilane and disilane mixture and accessory substance；
Monosilane and disilane mixture discharge reactor, are received by gas reception device；
Accessory substance is separated liquefied ammonia with accessory substance using filter with liquefied ammonia outflow reactor, and liquefied ammonia Jing is cold
But wet tank is returned to afterwards.
2. a kind of method that magnesium silicide method continuously prepares monosilane and disilane, it is characterised in that include with
Lower step：
The mixed liquor of liquefied ammonia and ammonium chloride is continuously squeezed into reactor from wet tank；
Magnesium silicide or Si-Mg alloy are added continuously in reactor；
Magnesium silicide or Si-Mg alloy start reaction after contacting with mixed liquor, generate monosilane and disilane mixing
Thing and accessory substance；
Monosilane and disilane mixture discharge reactor, are received by gas reception device；
Accessory substance is separated liquefied ammonia with accessory substance using filter with liquefied ammonia outflow reactor, liquefied ammonia and chlorine
Change ammonium and form mixed liquor, wet tank is returned to after cooling.
3. method according to claim 1 and 2, it is characterised in that
When raw material is magnesium silicide, the accessory substance is magnesium chloride hexammoniate, and methods described also includes：Will be with
Accessory substance magnesium chloride hexammoniate after Ammonia separation resolves into ammonia, and ammonia condensation forms liquefied ammonia, after cooling
Return to wet tank or mix with ammonium chloride, to be formed and return to wet tank after mixed liquor.
4. according to the method described in claim 3, it is characterised in that the decomposition of magnesium chloride hexammoniate is in drier
In carry out；
Preferably, the drier is propeller blade tube drier, including：Housing, axle, blade；
The axle is arranged in housing；
The blade is arranged on axle；
The propeller blade tube drier has the outlet of feed(raw material)inlet, product gas outlet and solid product；
Top to the end of the propeller blade tube drier has the temperature from room temperature to 300-450 DEG C
Gradient；
The product gas outlet, feed(raw material)inlet are arranged adjacent to the top of the drier, and the solid is produced
The end of the neighbouring drier of thing outlet is arranged.
5. method according to claim 1 and 2, it is characterised in that the gas reception device bag
Include backflow column scrubber and the first condenser；The monosilane and disilane mixture discharge reactor, and Jing is returned
The washing of stream column scrubber and the cooling of the first condenser, obtain thick monosilane and b silane gas.
6. method according to claim 1 and 2, it is characterised in that reaction mass is in liquefied ammonia
The time of staying is 0.1-10h；More preferably 0.1-3h.
7. method according to claim 1 and 2, it is characterised in that the purity of the liquefied ammonia is higher than
99.9%；More preferably purity is higher than 99.999%.
8. method according to claim 1 and 2, it is characterised in that the pressure in the reactor
For 0-2MPa, preferably 0.8-1.6MPa；Pressure in the wet tank is 0-0.8MPa.
9. method according to claim 1 and 2, it is characterised in that the temperature in the reactor
Control is between -50 DEG C of (- 40)；Preferably, the reaction in reactor is under alternating temperature temperature conditionss；More
Preferably, alternating temperature temperature conditionss are preferably：The direction that material is advanced along in reactor is heated up, and for gradient
Heat up；Most preferably, the direction advanced along material in reactor, temperature of reactor raises 30-60 DEG C；
The most preferably, reactor top temperature is (- 30)-(- 10) DEG C, and reactor terminal temperature is 20-40 DEG C.
10. a kind of magnesium silicide method continuously prepares the device (200) of monosilane and disilane, it is characterised in that
Including：
Wet tank (210), circulating pump (220), reactor (230), filter (240), cooling
Device (250), solid feed pot (260) and gas reception device (273)；
Reactor (230) is exported with liquid inlet, solid inlet, gas vent and suspension；
Filter (240) is with suspension inlet, liquid outlet and sludge outlet；
Outlet Jing circulating pumps (220) of wet tank (210) and the liquid inlet phase of reactor (230)
Even；
Solid feed pot (260) is connected with the solid inlet of reactor (230)；
The gas vent of reactor (230) is connected with gas reception device (273)；
The suspension outlet of reactor (230) is connected with the suspension inlet of filter (240)；
The liquid outlet of filter (240) is connected with the entrance of cooler (250)；
The outlet of cooler (250) is connected with the entrance of wet tank (210).
11. devices according to claim 10, it is characterised in that the gas reception device (273)
Including backflow column scrubber (270) and the first condenser (272)；Backflow column scrubber (270) entrance with
The gas vent of reactor (230) is connected, and outlet is connected with the first condenser (272).
12. devices according to claim 10, it is characterised in that described device (200) is also wrapped
Include drier (282) and the second condenser (284)；
Drier (282) is exported with feed(raw material)inlet, product gas outlet and solid product；
The feed(raw material)inlet of drier (282) is connected with the sludge outlet of filter (240), gaseous product
Outlet is connected with the entrance of the second condenser (284)；
The outlet of the second condenser (284) is connected with the entrance of wet tank (210)；
Preferably, the drier (282) is propeller blade tube drier, including：Housing (2821),
Axle (288), blade (289)；The axle (288) is arranged in housing (2821)；The blade (289)
It is arranged on axle (288)；Preferably, the product gas outlet (2823), feed(raw material)inlet (2822)
The top of the neighbouring drier (282) is arranged, and solid product outlet (2824) is neighbouring described dry
The end of dry device (282) is arranged.
13. devices according to claim 12, it is characterised in that drier (282) energy
Realize the thermograde from room temperature to 300-450 DEG C；Preferably, the propeller blade tube drier (282)
Top to end there is thermograde from room temperature to 300-450 DEG C.
14. devices according to claim 12, it is characterised in that the drier be divided into two sections or
Person's multi-stage series are constituted.
15. devices according to claim 10, it is characterised in that described device (200) is also wrapped
Include：Ammonium chloride liquefied ammonia prefabricated tanks (212)；The outlet of the second condenser (284) is prefabricated with ammonium chloride liquefied ammonia
The entrance of tank (212) is connected, outlet and the wet tank (210) of ammonium chloride liquefied ammonia prefabricated tanks (212)
Entrance be connected.
16. devices according to claim 10, it is characterised in that described device also adds including spiral
Material machine (262)；Solid feed pot (260) Jing self-conveyor feeds (262) are consolidated with reactor (230)
Body entrance is connected.
17. devices according to claim 10, it is characterised in that the reactor (230) is
Tubular reactor, preferably horizontal tube, vertical pipe type, coiled or U-shaped tubular reactor.
18. devices according to claim 17, it is characterised in that the tubular reactor is divided into two
Section or multi-stage series composition.
19. devices according to claim 10, it is characterised in that the reactor (230) is outward
Side is provided with external heat exchanger (231), and external heat exchanger (231) is provided with heat transferring medium entrance (232) and changes
Thermal medium outlet (233), heat transferring medium entrance (232) is positioned close to the outlet of reactor (230)
Side, heat transferring medium outlet (233) be positioned close to reactor (230) entrance side.
20. devices according to claim 10 or 17, it is characterised in that the reactor (230)
It is provided with least one radial agitator (235), including the first shaft (234) and is arranged on first and stirs
Mix the radial direction stirring vane (236) on axle (234)；
Or
Axial agitator (237), including the second shaft (238) are provided with the reactor (230)
With the axial stirring vane (239) being arranged on the second shaft (238).
21. devices according to claim 10, it is characterised in that the filter (240) is
Continuous filter；Preferably continuous pressing filter or screw extrusion filter；It is highly preferred that the company
Continuous pressing filter is pressurization rotary filter；Most preferably, the pressurization rotary filter is Barrate type
Filter, rotary drum type filter or collar plate shape filter；Filter medium in the filter (240) is excellent
Elect 10-1000 mesh stainless (steel) wires as.
22. devices according to claim 10, it is characterised in that in described device, by magnetic force
Drive.
Device of 23. employings as described in claim 10-22 is arbitrary is according to as described in claim 1-9 is arbitrary
Magnesium silicide method continuously prepare monosilane and the method for disilane continuously prepares monosilane and disilane.
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| CN201510753956.3A CN106672979B (en) | 2015-11-06 | 2015-11-06 | A kind of device and method that magnesium silicide method continuously prepares monosilane and disilane |
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| CN201510753956.3A CN106672979B (en) | 2015-11-06 | 2015-11-06 | A kind of device and method that magnesium silicide method continuously prepares monosilane and disilane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479211A (en) * | 2020-12-17 | 2021-03-12 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
| CN112661161A (en) * | 2020-12-28 | 2021-04-16 | 烟台万华电子材料有限公司 | Method for continuously producing high-order silane |
| CN112694091A (en) * | 2021-02-25 | 2021-04-23 | 刘振宇 | Electronic gas preparation system and method based on chip and intelligent manufacturing |
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| CN201686494U (en) * | 2010-03-18 | 2010-12-29 | 天津市泰亨气体有限公司 | Device for preparing silane |
| CN101928013A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Method for recycling ammonia in slurry of silane generator |
| CN102030332A (en) * | 2009-09-30 | 2011-04-27 | 鲍坚仁 | Application of byproducts in preparation of silane through magnesium silicide process |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
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|---|---|---|---|---|
| CN102030332A (en) * | 2009-09-30 | 2011-04-27 | 鲍坚仁 | Application of byproducts in preparation of silane through magnesium silicide process |
| CN201686494U (en) * | 2010-03-18 | 2010-12-29 | 天津市泰亨气体有限公司 | Device for preparing silane |
| CN101928013A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Method for recycling ammonia in slurry of silane generator |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479211A (en) * | 2020-12-17 | 2021-03-12 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
| CN112479211B (en) * | 2020-12-17 | 2022-10-04 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
| CN112661161A (en) * | 2020-12-28 | 2021-04-16 | 烟台万华电子材料有限公司 | Method for continuously producing high-order silane |
| CN112694091A (en) * | 2021-02-25 | 2021-04-23 | 刘振宇 | Electronic gas preparation system and method based on chip and intelligent manufacturing |
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| Publication number | Publication date |
|---|---|
| CN106672979B (en) | 2019-06-25 |
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