CN205222706U - System for continuous production hangs down impurity magnesium silicide - Google Patents
System for continuous production hangs down impurity magnesium silicide Download PDFInfo
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- CN205222706U CN205222706U CN201520884522.2U CN201520884522U CN205222706U CN 205222706 U CN205222706 U CN 205222706U CN 201520884522 U CN201520884522 U CN 201520884522U CN 205222706 U CN205222706 U CN 205222706U
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- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 53
- 239000012535 impurity Substances 0.000 title claims abstract description 16
- 238000010924 continuous production Methods 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 87
- 239000000463 material Substances 0.000 claims abstract description 69
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 238000004321 preservation Methods 0.000 claims description 36
- 230000004888 barrier function Effects 0.000 claims description 28
- 238000001816 cooling Methods 0.000 claims description 24
- 238000009825 accumulation Methods 0.000 claims description 16
- 230000008676 import Effects 0.000 claims description 5
- 230000003467 diminishing effect Effects 0.000 claims description 3
- 238000002955 isolation Methods 0.000 abstract description 7
- 230000001681 protective effect Effects 0.000 abstract description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 58
- 239000011777 magnesium Substances 0.000 description 54
- 229910052749 magnesium Inorganic materials 0.000 description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 28
- 239000007789 gas Substances 0.000 description 28
- 239000010703 silicon Substances 0.000 description 28
- 229910052710 silicon Inorganic materials 0.000 description 28
- 238000010586 diagram Methods 0.000 description 18
- 238000011049 filling Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 229910000077 silane Inorganic materials 0.000 description 5
- 239000011343 solid material Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 235000013312 flour Nutrition 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 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
- 238000010923 batch production Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000014509 gene expression Effects 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000011218 segmentation Effects 0.000 description 2
- 239000008247 solid mixture Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 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 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
The utility model discloses a system for continuous production hangs down impurity magnesium silicide, this system include reinforced jar, auger delivery reactor and receive the material jar, the auger delivery reactor includes: casing and the rotation axis of setting in the casing, be equipped with first feed inlet and discharge gate on the casing, be equipped with helical blade on the rotation axis, the auger delivery reactor includes the zone of heating, the zone of heating includes dominant reaction district and at least one isolation region, the auger delivery reactor has the material of messenger in local dynamic accumulational structure wherein in isolation region department, reinforced jar is equipped with the protective gas export, just reinforced jar sub -unit connection is to the first feed inlet of auger delivery reactor, receive the material jar and be equipped with protective gas inlet, just receive the discharge gate that the material jar was connected to the auger delivery reactor. The adoption system can realize that continuous production hangs down the impurity magnesium silicide.
Description
Technical field
The utility model relates to reactor, especially relates to the system of the low impurity magnesium silicide of a kind of continuous seepage.
Background technology
The history that magnesium silicide method prepares high purity silane and HIGH-PURITY SILICON is permanent, but is confined to small-scale production always.Trace it to its cause, mainly containing two: one is that technological process cannot realize continuously; Two is to realize real closed loop process route (referring to Chinese patent notification number CN102030332B).
Realize the magnesium silicide integrated process of operate continuously, first want continuous synthesis low impurity magnesium silicide powder.Magnesium silicide is generally synthesized by silicon and reactive magnesium, and magnesium infiltrates the lattice of silicon with magnesium vapor form and obtains product magnesium silicide.
The reaction of synthesizing magnesium silicide has following feature:
1) this is a remarkable thermopositive reaction.If can not remove reaction heat in time, the temperature of reaction bed is easy to be raised.During higher than 650 DEG C, the molecular ratio of the silicon magnesium in product will nonstoichiometry number 1:2, and follow-up yield when preparing silane is declined.
2) this reaction is that magnesium infiltrates the lattice of silicon with the form of magnesium vapor and obtains product magnesium silicide, but magnesium vapor easily loses, and that causes product to form departs from.In conventional methods where, in order to compensate the loss of magnesium vapor, the normally excessive 3-10% of magnesium.The excessive meeting of magnesium brings a series of problem.Such as, the consumption of ammonium chloride when product being used for subsequent production silane, can be increased, and then the amount of the ammonia causing needs to reclaim increases; Again such as, when electrolysis is carried out to the magnesium chloride produced when product being used for subsequent production silane, increase the power consumption etc. during electrolysis.And if magnesium is inexcessive, the reaction of silicon so usually will be caused incomplete.Residual silicon can enter into electrolyzer after series of process, has a negative impact, comprise and cause negative electrode passivation the electrolysis of magnesium chloride, reacts generate harmful silicon tetrachloride etc. with chlorine.
3) this reaction is the reaction that a volume increases.If can not provide enough expansion spaces and suitable stirring to material, product very easily lumps, and is unfavorable for that follow-up being used for prepares silane and other application.
The suitability for industrialized production of magnesium silicide can be divided into dpd mode: batch production and continuous seepage.The problem of batch production magnesium silicide is a lot, and the yield of magnesium silicide can only reach 90-95%, now less employing.
In 1963, HiroshiIshizuka (stoneman is great, DE1143190) reported helical feed formula reactor the earliest, achieves the continuous seepage of magnesium silicide, but this reactor exists the problem that magnesium vapor leaks, and yield and the purity of magnesium silicide are not so good.
CN101306818A proposes a kind of helical feed reactor of vertical layout, this reactor overcomes the problem that magnesium vapor leaks, but the vertical conveying of material needs to overcome a quick passage critical speed, and this rotating speed is quite large, and this forms contradiction with the time of the successive reaction reaching some hours.Meanwhile, the solid accumulation in this vertical reactor is too tight, and product very easily lumps.
CN201793377U proposes a kind of horizontal reactor, removes reaction heat by adding multiple method cooled in thermal jacket and tubular shaft of moving, and the temperature of reaction zone is controlled more accurate, but this application does not consider the problem that magnesium vapor leaks.
The technical scheme of CN102452653A adopts tank reactor, magnesium powder is joined in the silica flour of preheating, stirring, avoid local superheating and product caking by this process, but the leakage problem of magnesium vapor still exists, and raw material and grog mixing in retort, cause reaction efficiency not high.
CN202116325U adopts rotary kiln to carry out large scale continuous prod magnesium silicide, does not consider the problem that magnesium vapor and shielding gas leak.
Therefore, need a kind of new apparatus and method, the problem that magnesium vapor leaks can be solved, simple to operate, simultaneously the yield of magnesium silicide and purity good, do not lump, can continuous seepage.
Utility model content
The purpose of this utility model is the system providing the low impurity magnesium silicide of a kind of continuous seepage.
For reaching above-mentioned first object, the utility model adopts following technical proposals:
A system for the low impurity magnesium silicide of continuous seepage, this system comprises feed pot, helical feed reactor and rewinding tank;
Described helical feed reactor comprises: housing and the turning axle be arranged in housing; Housing is provided with the first opening for feed and discharge port; Turning axle is provided with screw-blade; Described helical feed reactor comprises heating zone; Described heating zone comprises main reaction region and at least one isolated area; Described helical feed reactor has the structure making material local dynamic station accumulation wherein at isolated area place;
Described feed pot is provided with shielding gas outlet, and the bottom of described feed pot is connected to the first opening for feed of helical feed reactor;
Described rewinding tank is provided with shielding gas import, and described rewinding tank is connected to the discharge port of helical feed reactor.
Further, described helical feed reactor is also provided with the second opening for feed; Preferably, the second opening for feed is connected with main reaction region.
Further, described reactor has barrier structure at isolated area place, and material is piled up at isolated area place local dynamic station.
Preferably, described barrier structure is selected from one or more in following structure:
1) turning axle is less than the structure of the pitch in other districts in the pitch of the screw-blade being positioned at isolated area place, referred to as narrow pitch helical blade structure.When rotating speed one timing of turning axle, other parts of axial velocity ratio of narrow pitch spiraling vane portions convey materials are slow, thus reactor is raised at the filling ratio of this part, cause material local accumulation, form isolated area.
2) turning axle is less than the structure of the blade diameter in other districts at the blade diameter of the screw-blade being positioned at isolated area place, is called for short minor diameter helical blade structure.Because the current rotating screw blade that needs of material is to provide power, adopts the sector-meeting of minor diameter helical-blade to reduce this power, just can cause material local accumulation, form isolated area.
3) turning axle is being positioned at the structure of isolated area place without screw-blade, referred to as plain shaft structure.Because the current rotating screw blade that needs of material is to provide power, when local is without eliminating this power during screw-blade, just can causes material local accumulation, forming isolated area.
4) turning axle and/or housing are being positioned at isolated area place and are being provided with the structure of baffle plate, and the structure of described baffle plate can meet material and pass through, but by area be less than other districts by area, referred to as baffle arrangement.The motion of material is obstructed at baffle plate place, and then produces solid accumulation before baffle plate, forms isolated area.
5) housing is less than the structure of the housing inner diameter in other districts at the housing inner diameter being positioned at isolated area place, referred to as little internal diameter shell structure.This structure can reduce the diameter of material channel, and filling ratio is raised, and causes material local accumulation, forms isolated area.Little internal diameter shell structure can be reduced by housing integral diameter to realize, and also can be to add convex structure at case inside to realize, and optional convex structure example is as ring texture.
6) housing is being positioned at the structure that isolated area place is the diminishing cone-shaped of internal diameter, referred to as tapered bore shell structure.This conical material road can make material pile up in cone, realizes isolation.Tapered bore shell structure can be reduced gradually by housing integral diameter to realize, and also can be to add the structure that can form tapered bore at case inside to realize, such as reducing ring.
More preferably, described baffle plate is around the first plectane that turning axle is arranged, diameter is less than housing inner diameter; Or to arrange around turning axle, surface is provided with second plectane in hole; Or lack type baffle plate around the circle that turning axle is arranged.
Further, described isolated area comprise the front isolated area before being arranged on main reaction region and/or be arranged on main reaction region after rear isolated area.
Further, described heating zone comprise set gradually preheating zone, main reaction region and heat preservation zone, and be arranged at least one isolated area before or after main reaction region.Preferably, described heating zone comprises the preheating zone set gradually, front isolated area, main reaction region, rear isolated area and heat preservation zone.
Described reactor can be arranged one or more, identical or different barrier structure, isolated area and/or rear isolated area before being formed in reactor.The barrier structure of front isolated area and rear isolated area can identical also can be different.Such as, when barrier structure can be set on housing, barrier structure is set on the rotary shaft simultaneously.
Further, described reactor also comprises the cooling zone after being arranged on heating zone.
Preferably, described reactor is for being horizontally disposed with or arranging horizontal by angle.The angle of altering reactor and horizontal plane can change the filling ratio of material in reactor, builds isolated area better.More preferably, the angle angle of reactor and horizontal plane is not more than 30 °.Described turning axle is parallel to housing and arranges.
Preferably, the length ratio of described preheating zone, main reaction region, heat preservation zone and cooling zone is: 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2.
Preferably, the length of described isolated area is not more than 5 housing inner diameter, is preferably 1 housing inner diameter to 3 housing inner diameter.
Preferably, described reactor is tube auger transport reactor.
Need because making, temperature control needs, isolate magnesium vapor needs or use at need, preferably tube auger transport reactor is divided into two sections or multi-stage series composition, the diameter of each section and from the angle of horizontal plane can identical also can be different, each segmentation of reactor does not change the selection of temperature parameter.
For reaching above-mentioned second object, adopt following technical proposals:
A method for the low impurity magnesium silicide of continuous seepage, silicon and magnesium enter reactor, and under shielding gas exists, successive reaction generates magnesium silicide, and wherein, material local dynamic station in reactor is piled up.
Reaction formula is:
2Mg+Si＝Mg
2Si。
Method of the present utility model, by being piled up by material local dynamic station in reactor, can be avoided the leakage of magnesium vapor, improve purity and the productive rate of product magnesium silicide powder.
Further, the filling ratio of described material in reactor is less than 0.5; Preferably, described filling ratio is not more than 0.3.Filling ratio is less than 0.5 and is especially not more than 0.3 silicon and magnesium can be made fully to react, enough spaces can also be provided for mass expanded simultaneously, heat transfer can be improved significantly again, temperature is controlled more accurate, thus avoid, because a large amount of heat release in reaction process and volume increase, impact is brought on the productive rate of product magnesium silicide, purity and form, the magnesium silicide fines of non-caking, low impurity can be obtained.
Further, the temperature of temperature higher than the reactor lower part region contacted with material of the reactor upper area do not contacted with material is controlled.Preferably, the temperature of reactor upper area is higher than the temperature in reactor lower part region more than 20 DEG C.When upper area is than lower region temperature height, magnesium vapor can be avoided to condense in the upper inside wall of reactor.The control to the upper area of reactor and the temperature of lower region is realized by employing electrically heated.
Further, before silicon and magnesium are entered reactor, by the preheating temperature in reactor to 400-900 DEG C, preferred 500-650 DEG C.
Further, described shielding gas is hydrogen or rare gas element.Preferably, the pressure of described shielding gas is (-0.1)-2MPa; Be more preferably (-0.1)-1.6MPa.
Further, described reactor comprises heating zone; Described heating zone comprises main reaction region and at least one isolated area; Described material is piled up at the isolated area place local dynamic station of reactor.Before silicon and magnesium are entered reactor, by the preheating temperature of the main reaction region of reactor to 400-900 DEG C, preferred 500-650 DEG C.
Further, described isolated area comprise the front isolated area before being arranged on main reaction region and/or be arranged on main reaction region after rear isolated area.
Further, described heating zone comprise set gradually preheating zone, main reaction region and heat preservation zone, and be arranged at least one isolated area before or after main reaction region.Preferably, described heating zone comprises the preheating zone set gradually, front isolated area, main reaction region, rear isolated area and heat preservation zone.Preheating zone can ensure water and other impurity of driving away absorption completely.In heat preservation zone, the amount of free magnesium is little, and most magnesium is reacted away in main reaction region, and a small amount of residual magnesium is wrapped among solid materials, is converted into magnesium silicide completely in heat preservation zone.
Further, described reactor also comprises the cooling zone after being arranged on heating zone.Material is naturally cooling in cooling zone, obtains the magnesium silicide powder loosened.
Further, first by silicon and magnesium mixing, afterwards silicon magnesium solid mixture is entered reactor through same opening for feed; Or silicon solid is entered reactor by the first opening for feed, and magnesium vapor enters reactor by the second opening for feed.Use magnesium vapor to replace magnesium powder as the raw material of synthesizing magnesium silicide, production cost can be reduced further, reduce oxide compound to the impact of subsequent reactions.
Further, material in preheating zone, time of stopping of main reaction region, heat preservation zone and cooling zone is than being 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2.
Further, described reactor is helical feed reactor, and this reactor comprises: housing and the turning axle be arranged in housing;
Housing is provided with the first opening for feed and discharge port;
Turning axle is provided with screw-blade;
Described reactor comprises heating zone;
Described heating zone comprises main reaction region and at least one isolated area;
Described reactor has the structure making material local dynamic station accumulation wherein at isolated area place.
Further, described reactor is also provided with the second opening for feed; Preferably, the second opening for feed is connected with main reaction region.
Further, described reactor has barrier structure at isolated area place, and material is piled up at isolated area place local dynamic station.
Preferably, described barrier structure is selected from the combination of a kind of or various structures in following structure:
1) turning axle is less than the structure of the pitch in other districts in the pitch of the screw-blade being positioned at isolated area place, referred to as narrow pitch helical blade structure.When rotating speed one timing of turning axle, other parts of axial velocity ratio of narrow pitch spiraling vane portions convey materials are slow, thus reactor is raised at the filling ratio of this part, cause material local accumulation, form isolated area.
2) turning axle is less than the structure of the blade diameter in other districts at the blade diameter of the screw-blade being positioned at isolated area place, is called for short minor diameter helical blade structure.Because the current rotating screw blade that needs of material is to provide power, adopts the sector-meeting of minor diameter helical-blade to reduce this power, just can cause material local accumulation, form isolated area.
3) turning axle is being positioned at the structure of isolated area place without screw-blade, referred to as plain shaft structure.Because the current rotating screw blade that needs of material is to provide power, when local is without eliminating this power during screw-blade, just can causes material local accumulation, forming isolated area.
4) turning axle and/or housing are being positioned at isolated area place and are being provided with the structure of baffle plate, and the structure of described baffle plate can meet material and pass through, but by area be less than other districts by area, referred to as baffle arrangement.The motion of material is obstructed at baffle plate place, and then produces solid accumulation before baffle plate, forms isolated area.
5) housing is less than the structure of the housing inner diameter in other districts at the housing inner diameter being positioned at isolated area place, referred to as little internal diameter shell structure.This structure can reduce the diameter of material channel, and filling ratio is raised, and causes material local accumulation, forms isolated area.Little internal diameter shell structure can be reduced by housing integral diameter to realize, and also can be to add convex structure at case inside to realize, and optional convex structure example is as ring texture.
6) housing is being positioned at the structure that isolated area place is the diminishing cone-shaped of internal diameter, referred to as tapered bore shell structure.This conical material road can make material pile up in cone, realizes isolation.Tapered bore shell structure can be reduced gradually by housing integral diameter to realize, and also can be to add the structure that can form tapered bore at case inside to realize, such as reducing ring.
More preferably, described baffle plate is around the first plectane that turning axle is arranged, diameter is less than housing inner diameter; Or to arrange around turning axle, surface is provided with second plectane in hole; Or lack type baffle plate around the circle that turning axle is arranged.
Described reactor can be arranged one or more, identical or different barrier structure, in reactor, form isolated area and/or rear isolated area before at least one.The barrier structure of front isolated area and rear isolated area can identical also can be different.Such as, when barrier structure can be set on housing, barrier structure is set on the rotary shaft simultaneously.
Further, described reactor also comprises the cooling zone after being arranged on heating zone.
Preferably, described reactor is for being horizontally disposed with or arranging horizontal by angle.The angle of altering reactor and horizontal plane can change the filling ratio of material in reactor, builds isolated area better.More preferably, the angle angle of reactor and horizontal plane is not more than 30 °.Described turning axle is parallel to housing and arranges.
Preferably, the length ratio of described preheating zone, main reaction region, heat preservation zone and cooling zone is: 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2.
Preferably, the length of described isolated area is not more than 5 housing inner diameter, is preferably 1 housing inner diameter to 3 housing inner diameter.
Preferably, described reactor is tube auger transport reactor.
Need because making, temperature control needs, isolate magnesium vapor needs or use at need, preferably tube auger transport reactor is divided into two sections or multi-stage series composition, the diameter of each section and from the angle of horizontal plane can identical also can be different, each segmentation of reactor does not change the selection of temperature parameter.
The beneficial effects of the utility model are as follows:
1, in system of the present utility model, helical feed reactor is by piling up the material local dynamic station at isolated area place, magnesium vapor is only existed in main reaction region, efficiently avoid the leakage of magnesium vapor in reaction process, silicon residual in product and the amount of magnesium are far below the amount of silicon residual in commercially available chemical pure magnesium silicide and magnesium.
2, system of the present utility model can realize the magnesium silicide fines of the low impurity of continuous seepage.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, embodiment of the present utility model is described in further detail.
Fig. 1 is the schematic diagram of a kind of embodiment of helical feed reactor of the present utility model;
Fig. 2 is the isolated area schematic diagram that narrow pitch helical blade structure builds;
Fig. 3 is the isolated area schematic diagram that baffle arrangement builds;
Fig. 4 is the isolated area schematic diagram that minor diameter helical blade structure builds;
Fig. 5 is the isolated area schematic diagram that plain shaft structure builds;
Fig. 6 is the isolated area schematic diagram that a kind of embodiment of little internal diameter shell structure builds;
Fig. 7 is the isolated area schematic diagram that the another kind of embodiment of little internal diameter shell structure builds;
Fig. 8 is the isolated area schematic diagram that a kind of embodiment of tapered bore shell structure builds;
Fig. 9 is the isolated area schematic diagram that the another kind of embodiment of tapered bore shell structure builds;
Figure 10 is the schematic diagram of the another kind of embodiment of helical feed reactor of the present utility model;
Figure 11 is the XRD figure spectrum of the magnesium silicide product of embodiment 3 gained;
Figure 12 is the XRD figure spectrum of commercially available chemical pure (99.5%) magnesium silicide.
Embodiment
In order to be illustrated more clearly in the utility model, below in conjunction with preferred embodiments and drawings, the utility model is described further.For knowing and being convenient to understand parts, each several part not drawn on scale in accompanying drawing.Parts similar in accompanying drawing represent with identical Reference numeral, and dotted line is used for representing region.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive below, protection domain of the present utility model should do not limited with this.
Fig. 1 shows a kind of embodiment of helical feed reactor 150 of the present utility model.
A kind of helical feed reactor 150, this reactor 150 comprises: housing 151 and the turning axle 152 be arranged in housing 151;
Housing 151 is provided with the first opening for feed 130 and discharge port 131; Feed pot 120 is connected with the first opening for feed 130, is provided with shielding gas outlet 110; Discharge port 131 is connected with rewinding tank 121, and rewinding tank 121 is provided with shielding gas import 111;
Turning axle 152 is provided with screw-blade 153, drives through motor 140;
Described reactor 150, between the first opening for feed 130 and discharge port 131, comprises heating zone 160 and cooling zone 165; Described heating zone 160 comprise set gradually preheating zone 161, front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164;
Described reactor 150 has barrier structure at isolated area place, and material is piled up at isolated area place local dynamic station.The dynamic accumulation of the material at front isolated area 170 place is by preheating zone and main reaction region isolation; The dynamic accumulation of the material at rear isolated area 171 place is by main reaction region and heat preservation zone isolation; This isolation makes magnesium vapor only exist in main reaction region.
Described reactor 150 is tube auger transport reactor, places horizontal by being not more than 30 ° of angles.Turning axle 152 is parallel to housing 151 and arranges.The length ratio of the preheating zone 161 of reactor, main reaction region 162, heat preservation zone 164 and cooling zone 165 is: 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2, the length of front isolated area 170 and rear isolated area 171 is all not more than 5 housing inner diameter, is preferably 1 housing inner diameter to 3 housing inner diameter.
As shown in Figure 2, the isolated area schematic diagram built when be barrier structure being narrow pitch helical blade structure.In figure, 180 represent narrow pitch helical blade structure, 172 isolated areas built for narrow pitch helical blade structure.
As shown in Figure 3, the isolated area schematic diagram built when be barrier structure being baffle arrangement.In figure, 181 represent baffle arrangement, 173 isolated areas built for baffle arrangement.Baffle plate 181 can have different shapes, such as arrange around turning axle 152, diameter is less than the first plectane 181a of housing 151 internal diameter; Or arrange around turning axle 152, surface is provided with the second plectane 181b in hole; Or lack type baffle plate 181c around the circle that turning axle 152 is arranged.
As shown in Figure 4, the isolated area schematic diagram built when be barrier structure being minor diameter helical blade structure.In figure, 182 represent minor diameter helical blade structure, 174 isolated areas built for minor diameter helical blade structure.
As shown in Figure 5, the isolated area schematic diagram built when be barrier structure being plain shaft structure.In figure, 183 represent plain shaft structure, 175 isolated areas built for plain shaft structure.
As shown in Figure 6, the isolated area schematic diagram built when be barrier structure being a kind of embodiment of little internal diameter shell structure.In figure, housing integral diameter reduces and realizes little internal diameter shell structure by 184 expressions, and 176 is housing integral diameter is reduced the isolated area realizing little internal diameter shell structure and build.
As shown in Figure 7, the isolated area schematic diagram built when be barrier structure being the another kind of embodiment of little internal diameter shell structure.In figure, 185 represent that adding ring texture at case inside realizes little internal diameter shell structure, and 177 is add at case inside the isolated area that ring texture realizes little internal diameter shell structure structure.
As shown in Figure 8, the isolated area schematic diagram built when be barrier structure being a kind of embodiment of tapered bore shell structure.In figure, housing integral diameter reduces and realizes tapered bore shell structure by 186 expressions gradually, and 178 is housing integral diameter is reduced gradually the isolated area realizing tapered bore shell structure and build.
As shown in Figure 7, the isolated area schematic diagram built when be barrier structure being the another kind of embodiment of tapered bore shell structure.In figure, 187 represent that adding reducing ring at case inside realizes tapered bore shell structure, and 179 is add at case inside the isolated area that reducing ring realizes tapered bore shell structure structure.
This reactor with an opening for feed is applicable to, first by silicon and magnesium mixing, afterwards silicon magnesium solid mixture be entered the pattern of reactor through same opening for feed.Silicon solid and magnesium solid are first joined in blender (not shown) by stoicheiometry, after fully stirring mixed and shielding gas displacement, joins in feed pot 120, close the valve between blender and feed pot 120.
Figure 10 shows the another kind of embodiment of helical feed reactor 150 of the present utility model, and this embodiment is with the difference of front a kind of reactor: also comprise the second opening for feed 190 be connected with main reaction region 162; Second opening for feed 190 is connected with air lift still 191, is contained with liquid magnesium 193 in air lift still 191, and the thin stainless steel tube 192 of liquid magnesium shielding gas through being provided with shielding gas valve 194 passes in liquid nitrogen 193.This reactor with two opening for feeds is that silicon solid is entered reactor by the first opening for feed, and magnesium vapor enters reactor by the second opening for feed.
Embodiment 1
A method for the low impurity magnesium silicide of continuous seepage, adopts system as shown in Figure 1, comprises the steps:
1, open vacuum system, after the vacuum tightness of helical feed reactor 150 reaches requirement, (be generally-0.099MPa), close vacuum pipe, open shielding gas import 111, in helical feed reactor, pass into shielding gas; This step in triplicate; Pass into shielding gas, keep;
2, by the preheating temperature of front for helical feed reactor 150 isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 to 400-900 DEG C, the temperature of the upper area 163 (not having solid materials district) of main reaction region 162 is higher more than 20 DEG C than the temperature of the lower region (having solid materials district) of main reaction region 162, keeps;
3, silica flour, magnesium powder two kinds of materials are joined in blender by stoicheiometry, after fully stirring mixed and shielding gas displacement, join in feed pot 120, close the valve between blender and feed pot 120; Afterwards silicon magnesium compound material is added helical feed reactor 150.Silicon magnesium material through preheating zone 161, construct front isolated area 170 laggard enter main reaction region 162, main reaction region silicon magnesium material reaction generate magnesium silicide, the silicon magnesium material of non-complete reaction and the magnesium silicide of generation are constructed rear isolated area 171, are then entered heat preservation zone 164 and cooling zone 165, obtain product magnesium silicide powder at rewinding tank 121.
Material in preheating zone 161, main reaction region 162, heat preservation zone 164, different with the time that cooling zone 165 stops, time of stopping in above-mentioned district is than being 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2.In reaction, the filling ratio of silicon magnesium material in helical feed reactor is less than 0.5; Preferred filling ratio is no more than 0.3.In whole reaction process, shielding gas is hydrogen or rare gas element, and the pressure of shielding gas is-0.1-2MPa; Preferred pressure is-0.1-1.6MPa.
Embodiment 2
A method for the low impurity magnesium silicide of continuous seepage, adopts system as shown in Figure 10, comprises the steps:
1, open vacuum system, reach after requirement (being generally-0.099MPa) until helical feed reactor 150 vacuum tightness, close vacuum pipe, open shielding gas import 111, in helical feed reactor 150, pass into shielding gas; This step in triplicate; Pass into shielding gas, keep;
2, by the preheating temperature of front for helical feed reactor isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 to 400-900 DEG C, the temperature of the upper area 163 (not having solid materials district) of main reaction region 162 is higher more than 20 DEG C than the temperature of the lower region (having solid materials district) of main reaction region 162, keeps; And MAGNESIUM METAL is added air lift still 191;
3, open the vacuum system of air lift still 191, reach after requirement (being generally-0.099MPa) until air lift still 191 vacuum tightness, close vacuum pipe, in air lift still, pass into shielding gas; This step in triplicate;
4, by air lift still 191 preheating, keep;
5, silica flour is joined feed pot 120 under protective atmosphere;
6, silica flour is entered helical feed reactor 150, isolated area 170 before building behind preheating zone 161;
7, air lift still shielding gas valve 194 is opened; liquid magnesium 193 air lift in air lift still 191 becomes magnesium vapor; enter main reaction region 162 by the second opening for feed 190 and start reaction; rear isolated area 171 constructed by the magnesium silicide generated and the silicon magnesium material of non-complete reaction; then enter heat preservation zone 164 and cooling zone 165, obtain product magnesium silicide powder at rewinding tank 121.
Material in preheating zone 161, main reaction region 162, heat preservation zone 164, different with the time that cooling zone 165 stops, time of stopping in above-mentioned district is than being 0-2:0.01-4:0-4:0-4; Be preferably 0.5:1-2:1-2:1-2.In reaction, the filling ratio of silicon magnesium material in helical feed reactor is less than 0.5; Preferred filling ratio is no more than 0.3.In whole reaction process, shielding gas is hydrogen or rare gas element, and the pressure of shielding gas is-0.1-2MPa; Preferred pressure is-0.1-1.6MPa.
Embodiment 3
With embodiment 1, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 temperature be 550 DEG C;
Silicon, magnesium two kinds of materials in molar ratio 1:2 join blender;
Barrier structure is the narrow pitch helical blade structure shown in Fig. 2.
The time that material stops in preheating zone 161 is about 0.5 hour, is about 1.5 hours in main reaction region 162 residence time, is about 1.5 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour.
Figure 11 is the XRD figure spectrum of the magnesium silicide powder-product of embodiment 3 gained; Figure 12 is the XRD figure spectrum of commercially available chemical pure (99.5%) magnesium silicide.Can find out, silicon residual in the magnesium silicide product of embodiment 3 and the amount of magnesium are all far below the amount of silicon residual in commercially available chemical pure (99.5%) magnesium silicide and magnesium.
Illustrate and adopt method of the present utility model continuously, uninterruptedly can produce low impurity magnesium silicide powder.
Embodiment 4
With embodiment 2, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 temperature be 650 DEG C;
Air lift still 191 is preheating to 660 DEG C makes MAGNESIUM METAL melt;
Shielding gas is hydrogen;
Barrier structure is the first plectane 181a in the baffle arrangement shown in Fig. 3.
The time that material stops in preheating zone 161 is about 0.5 hour, is about 1 hour in main reaction region 162 residence time, is about 2 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 2 hours.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 5
With embodiment 1, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 temperature be 600 DEG C;
The time that material stops in preheating zone 161 is about 0.75 hour, is about 1.5 hours in main reaction region 162 residence time, is about 1.5 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1.5 hours;
Front isolated area adopts the minor diameter helical blade structure shown in Fig. 4, and rear isolated area adopts the plain shaft structure shown in Fig. 5.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 6
With embodiment 1, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 heating temperatures to 480 DEG C;
The time that material stops in preheating zone 161 is about 1 hour, is about 3 hours in main reaction region 162 residence time, is about 2 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour;
Barrier structure is the plain shaft structure shown in Fig. 5.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 7
With embodiment 1, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 heating temperatures to 560 DEG C;
The time that material stops in preheating zone 161 is about 0.5 hour, is about 2 hours in main reaction region 162 residence time, is about 1.5 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour;
Barrier structure is the little internal diameter shell structure shown in Fig. 6.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 8
With embodiment 2, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 heating temperatures to 620 DEG C;
The time that material stops in preheating zone 161 is about 0.5 hour, is about 1.5 hours in main reaction region 162 residence time, is about 1 hour in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour;
Barrier structure is the little internal diameter shell structure shown in Fig. 7.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 9
With embodiment 2, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 heating temperatures to 800 DEG C;
The time that material stops in preheating zone 161 is about 0.25 hour, is about 1 hour in main reaction region 162 residence time, is about 1 hour in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour;
Front isolated area adopts tapered bore shell structure as shown in Figure 8, and rear isolated area adopts tapered bore shell structure as shown in Figure 9.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Embodiment 10
With embodiment 1, wherein:
Keep front isolated area 170, main reaction region 162, rear isolated area 171 and heat preservation zone 164 heating temperatures to 520 DEG C;
The time that material stops in preheating zone 161 is about 0.5 hour, is about 2 hours in main reaction region 162 residence time, is about 1.5 hours in heat preservation zone 164 residence time, and the time stopped in cooling zone 165 is about 1 hour;
Front isolated area adopts little internal diameter shell structure and baffle arrangement combination to build, and rear isolated area adopts tapered bore shell structure and local plain shaft structure combination to build.
After tested, residual in magnesium silicide product silicon is almost consistent with embodiment 3 with the amount of magnesium.
Obviously; above-described embodiment of the present utility model is only for the utility model example is clearly described; and be not the restriction to embodiment of the present utility model; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to the technical solution of the utility model the apparent change of extending out or variation be still in the row of protection domain of the present utility model.
Claims (10)
1. a system for the low impurity magnesium silicide of continuous seepage, is characterized in that, described system comprises feed pot (120), helical feed reactor (150) and rewinding tank (121);
Described helical feed reactor (150) comprising: housing (151) and the turning axle (152) be arranged in housing (151); Housing (151) is provided with the first opening for feed (130) and discharge port (131); Turning axle (152) is provided with screw-blade (153); Described helical feed reactor (150) comprises heating zone (160); Described heating zone (160) comprises main reaction region (162) and at least one isolated area; Described helical feed reactor (150) has the structure making material local dynamic station accumulation wherein at isolated area place;
Described feed pot (120) is provided with shielding gas outlet (110), and the bottom of described feed pot (120) is connected to first opening for feed (130) of helical feed reactor (150);
Described rewinding tank (121) is provided with shielding gas import (111), and described rewinding tank (121) is connected to the discharge port (131) of helical feed reactor (150).
2. system according to claim 1, is characterized in that, described helical feed reactor (150) is also provided with the second opening for feed (190); Second opening for feed (190) is connected with main reaction region (162).
3. system according to claim 1 and 2, is characterized in that, described helical feed reactor (150) has barrier structure at isolated area place, and material is piled up at isolated area place local dynamic station.
4. system according to claim 3, is characterized in that, described barrier structure be selected from following structure one or more:
1) turning axle (152) is less than the structure of the pitch in other districts in the pitch of the screw-blade (153) being positioned at isolated area place;
2) turning axle (152) is less than the structure of the blade diameter in other districts at the blade diameter of the screw-blade (153) being positioned at isolated area place;
3) turning axle (152) is being positioned at the structure of isolated area place without screw-blade (153);
4) turning axle (152) and/or housing (151) are being positioned at isolated area place and are being provided with the structure of baffle plate (181);
5) housing (151) is less than the structure of the housing inner diameter in other districts at the housing inner diameter being positioned at isolated area place;
6) housing (151) is being positioned at the structure that isolated area place is the diminishing cone-shaped of internal diameter.
5. system according to claim 1 and 2, it is characterized in that, described isolated area comprises the front isolated area (170) be arranged on before main reaction region (160) and/or the rear isolated area (171) be arranged on after main reaction region (162).
6. system according to claim 1 and 2, it is characterized in that, described heating zone (160) comprise set gradually preheating zone (161), main reaction region (162) and heat preservation zone (164), and be arranged at least one isolated area before or after main reaction region (162).
7. system according to claim 1 and 2, is characterized in that, described reactor (150) also comprises the cooling zone (165) be arranged on after heating zone (160).
8. system according to claim 1 and 2, is characterized in that, described reactor (150) is horizontal by angle, and angle angle is not more than 30 °.
9. system according to claim 6, it is characterized in that, the length ratio of described preheating zone (161), main reaction region (162), heat preservation zone (164) and cooling zone (165) is: 0-2:0.01-4:0-4:0-4.
10. system according to claim 1 and 2, is characterized in that, the length of described isolated area is not more than 5 housing inner diameter.
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| CN201520884522.2U CN205222706U (en) | 2015-11-06 | 2015-11-06 | System for continuous production hangs down impurity magnesium silicide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597025A (en) * | 2017-09-26 | 2018-01-19 | 中天储能科技有限公司 | A kind of silicon monoxide quantity-produced apparatus |
| CZ307267B6 (en) * | 2017-04-25 | 2018-05-02 | Ústav Chemických Procesů Av Čr, V. V. I. | A method of preparation of magnesium silicide at a low temperature |
-
2015
- 2015-11-06 CN CN201520884522.2U patent/CN205222706U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ307267B6 (en) * | 2017-04-25 | 2018-05-02 | Ústav Chemických Procesů Av Čr, V. V. I. | A method of preparation of magnesium silicide at a low temperature |
| CN107597025A (en) * | 2017-09-26 | 2018-01-19 | 中天储能科技有限公司 | A kind of silicon monoxide quantity-produced apparatus |
| CN107597025B (en) * | 2017-09-26 | 2024-04-30 | 中天储能科技有限公司 | Equipment device for continuous production of silicon monoxide |
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