CN103183324B - Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar - Google Patents
Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar Download PDFInfo
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- CN103183324B CN103183324B CN201310024134.2A CN201310024134A CN103183324B CN 103183324 B CN103183324 B CN 103183324B CN 201310024134 A CN201310024134 A CN 201310024134A CN 103183324 B CN103183324 B CN 103183324B
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- silicon nitride
- nitrogen
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- waste mortar
- silica flour
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 47
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 46
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 229910021419 crystalline silicon Inorganic materials 0.000 title claims abstract description 32
- 239000002699 waste material Substances 0.000 title claims abstract description 32
- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 31
- 239000000843 powder Substances 0.000 title claims abstract description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 40
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 235000013312 flour Nutrition 0.000 claims description 41
- 238000012545 processing Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 9
- 238000005245 sintering Methods 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 238000012856 packing Methods 0.000 claims description 8
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 239000004576 sand Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 4
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- -1 Silicon imide Chemical class 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 4
- 238000010574 gas phase reaction Methods 0.000 description 4
- 238000006396 nitration reaction Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 229910052572 stoneware Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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- Ceramic Products (AREA)
Abstract
A unit for preparing a silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar comprises an entrained-flow reactor 1, a nitrogen plasma igniter 13, a pressure controller 2, a tunnel kiln 3, a kiln car 4, a dryer 5, a silica powder storage bin 6, a silica powder pneumatic conveyer 7, an Si3N4 pneumatic conveyer 8, an Si3N4 storage bin 9, a product measurement packaging device 10, an air-separation nitrogen-making device 11, an automatic control system 12, and related pipelines, valves and instruments, wherein the entrained-flow reactor 1, the pressure controller 2, the tunnel kiln 3 and the kiln car 4 are core or key equipment of the unit, and others are equipment capable of being matched with mature technologies in the market; and the silica powder and nitrogen recovered by the crystalline silicon processed waste mortar are taken as the raw materials, and the nitrogen is taken as the raw material and a heat transfer carrier to produce a silicon carbide ceramic material combining silicon nitride micro powder and silicon nitride.
Description
Technical field
The present invention relates to the unit that silicon nitride product prepared by a kind of crystalline silicon processing waste mortar recovery silica flour, belong to solar-energy photo-voltaic cell crystalline silicon processing waste field of comprehensive utilization.
Background technology
Silicon nitride is the engineering ceramic material of a kind of advanced person, there is high room temperature and hot strength, high rigidity, resistance to abrasion, oxidation-resistance and good heat shock resistance and mechanical shock performance, thought high comprehensive performance in structural ceramics field by material supply section educational circles, be hopeful a kind of novel material that alternative nickel-base alloy obtains widespread use in high-tech, high-temperature field most.
Beta-silicon nitride powder synthesis technique is generally:
Silica flour Direct-Nitridation 3Si+2N
2=Si
3n
4
Silicon imide gas-phase reaction 3SiCl
4+ 4NH
3=Si
3n
4+ 12HCl
Carbothermal reduction-nitridation 3SiO
2+ 6C+2N2=Si
3n
4+ 6CO
Wherein silica flour Direct-Nitridation prepares the technique that beta-silicon nitride powder develops the earliest, and be also a kind of method be most widely used at present, this method is relatively simple, low price, use raw material is crystalline silicon, belongs to intervalization production, product is block, has to pass through ball milling and just can obtain micro mist; Silicon imide gas-phase reaction, needs special initial feed, expensive, and reaction process produces a large amount of hydrogenchloride, has particular requirement to equipment, and manufacturing cost is high, but product purity is high, fine size and evenly; Carbothermal reduction-nitridation reaction process, raw material is easy to get, energy consumption is high, pollution is heavy, and apparatus and process is complicated;
Crystalline silicon processing waste mortar be formed in solar-energy photo-voltaic cell process of manufacture be mixed with 40 ~ 50%PEG (polyoxyethylene glycol cutting liquid), 45 ~ 30%SiC (cutting abrasive material), the iron powder (line of cut wearing and tearing) of 1 ~ 3%, the quaternary mixture system of 14 ~ 17%Si powder (crystalline silicon abrasive dust).
Applicant paid close attention to the process problem of solar-energy photo-voltaic cell crystalline silicon processing waste mortar from 2006, the optimized recovery and utilization technology of exploratory development.Propose the application for a patent for invention of " the waste mortar formed by processing photovoltaic cell crystalline silicon comprehensive treating process novel method " of application number 201110101064.7 on April 22nd, 2011, within 2011, within 08 month 12 days, propose the application for a patent for invention of application number 201110238197.9 " comprehensive treatment technology of waste mortar in processing of photovoltaic crystalline silicon ", carried out supplementing to previous patent application perfect.On June 26th, 2012, application number 201110238197.9 " comprehensive treatment technology of waste mortar in processing of photovoltaic crystalline silicon " was that 201210207989.4 " the crystalline silicon processing waste mortar comprehensive treatment techniques without sewage and solid waste discharge " propose to contain SiC, Si binary sand for raw material for right of priority proposes application number again, utilized the technical scheme of air flow bed Nitration synthesis nano-silicon nitride; Conduct in-depth research the Industrialized processing technique of this scheme afterwards, invention devises " utilizing crystalline silicon processing waste mortar recovery silica flour to prepare the unit of silicon nitride product "
Summary of the invention
The present invention on the basis of the silicon nitride production-process systems such as synthetic study silicon nitride silica flour Direct-Nitridation, silicon imide gas-phase reaction, to the Supplementary and perfect of the air flow bed Nitration synthesis nitride process of the application for a patent for invention of application number 201210207989.4 " the crystalline silicon processing waste mortar comprehensive treatment technique without sewage and solid waste discharge ".
The object of this invention is to provide a kind of advantage combining silica flour Direct-Nitridation and silicon imide gas-phase reaction two Technologies, eliminate simultaneously they separately defect reclaim with crystalline silicon processing waste mortar silica flour to prepare silicon nitride product unit as raw material.
The object of the present invention is achieved like this: produce unit by entrained-flow reactor, nitrogen gas plasma lighter for ignition, pressure controller, tunnel furnace, kiln car, drying machine, silica flour feed bin, silica flour air conveyor, Si
3n
4air conveyor, Si
3n
4feed bin, ganging of products packing plant, nitrogen-making device, robot control system(RCS) and relevant ducts, valve, instrument are formed; The silica flour reclaimed with crystalline silicon processing waste mortar and nitrogen, for raw material, take nitrogen as delivery vehicles, produce silicon nitride powder and silicon nitride combined silicon carbide stupalith.
Raw material for the production of silicon nitride powder is the silicon powder utilizing crystalline silicon processing waste mortar to reclaim, and its composition is Si>=80-95%, SiC≤20-5%, Fe
2o
3≤ 0.1%.
Raw material for the production of silicon nitride powder is containing N
2the nitrogen of 98 ~ 99.99%, output pressure 0.1 ~ 1.0MPa, the throughput of supporting nitrogen-making device is 2 ~ 8 times of actual nitrogenize consumption, to meet unit raw material and heat delivery needs.
The synthesis of silicon nitride powder completes in the nucleus equipment-entrained-flow reactor of unit; Air flow bed operating pressure 0.1 ~ 1.6MPa, aspect ratio 3 ~ 10: 1.
Raw material for the manufacture of silicon nitride combined silicon carbide stupalith blank is the binary sand that crystalline silicon processing waste mortar reclaims, and tool composition is Si=40--20%, SiC=60--80%, Fe
2o
3≤ 0.1%.
That the reaction nitrogen that entrained-flow reactor is discharged, temperature 1200--1600 DEG C, pressure 0.01--0.10MPa contain a small amount of silicon nitride powder provides for the production of the energy of silicon nitride combined silicon carbide stupalith sintering and nitrogen.
The reaction sintering of silicon nitride combined silicon carbide stupalith completes in the key equipment-tunnel furnace of this unit; Tunnel furnace operating pressure≤0.1MPa, working sections amass be air flow bed sectional area 0.5--4 doubly, length be air flow bed height 5--20 doubly; Tunnel like sintered channels is combined to form with supporting kiln car.(separate case application)
The nitrogen transmitting device connecting entrained-flow reactor and tunnel furnace is pressure controller, its front end is provided with carries out pressure controlled automatically controlled valve according to entrained-flow reactor processing requirement, rear end is provided with the air distributor with tunnel kiln sintering process matching, pressure controller shell is metal shell, and liner can bear the lagging material of 1200--1600 DEG C.
Except said flow bed bioreactor, tunnel furnace, kiln car, the necessary specialized designs manufacture of pressure controller, all the other comprise nitrogen gas plasma lighter for ignition, drying machine, silica flour feed bin, silica flour air conveyor, Si
3n
4air conveyor, Si
3n
4feed bin, ganging of products packing plant, nitrogen-making device, robot control system(RCS) and relevant ducts, valve, instrument all can, according to unit design ability, select market-ripe device element supporting.
Hereby in conjunction with the accompanying drawings and embodiments the present invention is further described.
Accompanying drawing explanation
Ordering-the figure reclaims silica flour with crystalline silicon processing waste mortar to prepare silicon nitride product crew qiting figure.
In figure, arrow represents the pipeline connecting production line relevant device, the material of conveying in the character representation pipeline above it, and arrow represents material traffic direction, pipeline is equipped with corresponding by-pass valve control; Circle represents the instrument installed on a production line, and P is pressure instrumentation, TT is temperature instrument, and what be connected with two dot chain line with robot control system(RCS) 11 is that teletransmission controls detecting instrument, and without line is in-site installation instrument; Figure number 1 is this unit nucleus equipment---entrained-flow reactor (separate case application), 2 be pressure controller, 3 for unit key equipment---tunnel furnace (separate case application), 4 is the supporting kiln car of tunnel furnace (separate case application), 5 be silica powder drying machine, 6 be silica flour feed bin, 7 be silica flour air conveyor, 8 be Si
3n
4air conveyor, 9 is Si
3n
4the silicon nitride combined silicon carbide ceramic component of feed bin, 10 ganging of products packing plants, 11 are nitrogen-making device, 12 to be robot control system(RCS), 13 be plasma igniter, 14 pressure controllers control flashboards, 15 to be under meter, 16 be tunnel kiln sintering.
Embodiment
Be below specific embodiments of the invention, but method of the present invention is also not exclusively limited, those skilled in the art can change step wherein as required or omit.
Embodiment 1:
Prepare shown in the crew qiting figure of silicon nitride product as reclaimed silica flour with crystalline silicon processing waste mortar: nitrogen-making device 11 is nitrogen output 2000Nm processed
3/ h, purity N
299.9%, the swing adsorption nitrogen producing apparatus of output pressure 0.6MPa, the nitrogen produced is through under meter 15 adjust flux, enter silica flour air conveyor 7, by gas-solid mass ratio 1: 1 ratio of mixture with the speed of 1t/h be stored in silica flour feed bin 6 containing Si84%, SiC16% silica flour, in spray people reaction gas flow bed bioreactor 1, lighted a fire by nitrogen gas plasma 13, trigger the N in reactor
2, Si, SiC form the reaction of self-propagating Nitration synthesis, react according to 3SiC+2N
2=Si
3n
4+ 3C+62000KJ and 3Si+2N
2=Si
3n
4+ 751570KJ two nitrogenizing reaction equations carry out, and exothermic heat of reaction can reach 2220kw, and temperature of reaction can be made to reach 2680 DEG C; Optimum operating condition 1300--1450 DEG C is being reacted for controlling working temperature in entrained-flow reactor, the nitrogen of required 2 ~ 8 times is reacted along reactor wall side direction spray people, in reactor 1, form eddy flow, shielding gas flow bed bioreactor 1, ensures the complete reaction of Si, SiC simultaneously; The Si of synthesis
3n
4be gathered in reactor bottom water cooler, be cooled to 600 ~ 800 DEG C; With pressurized air with the ratio of mixture of gas-solid mass ratio 1: 50 by Si
3n
4air conveyor 8 is transported in product feed bin 9, utilizes the oxygen in air simultaneously, reacts with the carbon of SiC nitrogenize by-product, and the de-C of gasification, by ganging of products packing plant 10 metering packing, puts in storage for sale; Reaction residue nitrogen carries the energy of 500--700kw and a small amount of reaction product through pressure controller 2 with the high temperature of 1300--1450 DEG C, by regulating the keying amplitude adjusted entrained-flow reactor internal pressure of pressure-controlling flashboard 14, enter in tunnel furnace 3, utilize high temperature N
2complete in tunnel furnace the nitrogenizing reaction sintering of the three-dimensional foam strainer prepared with SiC, Si binary sand be contained on kiln car 4, and utilize the remaining nitrogen of nitrogen-making device to cool at tunnel furnace cooling section, form silicon nitride combined silicon carbide three-dimensional foam porcelain filter 16; The waste gas that tunnel furnace is discharged is temperature at the nitrogen of 300 ~ 600 DEG C, silica flour filtration cakes torrefaction machine 5 is entered by pipeline, for the silica flour filter cake of drying from waste mortar treatment system, dried silica flour enters silica flour feed bin 6, and separating off nitrogen G&W vapor vent is discharged.
Prepared by Nitrogen plant using air separation process 11 contains N
2the nitrogen of more than 99.9% is the important factor that maintenance unit normally runs, carry and reactive material is provided, conveying reaction raw materials, derive the multitask such as heat of reaction, dry reaction raw material, this unit adopts swing adsorption nitrogen producing apparatus, and nitrogen power consumption is low, starts the cycle short, level of automation is high, can realize unmanned; Self-con-tained unit 12 is responsible for the production of whole production line, safe Automated condtrol and operation.
Embodiment 2:
Prepare shown in the crew qiting figure of silicon nitride product as reclaimed silica flour with crystalline silicon processing waste mortar: nitrogen-making device 11 is nitrogen output 3000Nm processed
3/ h, purity N
299.5%, the compression air separation device of pressure 0.6MPa, is producing 3000Nm
3can the nearly 800Nm of by-product while/h nitrogen
3/ h oxygen is used for export trade, can eat up part of part nitrogen cost; The passing nitrogen produced is through under meter 15 adjust flux, enter silica flour air conveyor 7, Si92%, SiC8% silica flour is contained with the speed of 1.51t/h being stored in the dried of silica flour feed bin 6 by the ratio of mixture of gas-solid mass ratio 1: 1, in spray people entrained-flow reactor 1, lighted a fire by nitrogen gas plasma 13, N2, Si, the SiC triggered in reactor forms Nitration synthesis reaction, according to 3SiC+2N
2=Si
3n
4+ 3C+62000KJ and 3Si+2N
2=Si
3n
4+ 751570KJ two nitrogenizing reaction equations form self-propagating thermopositive reaction, exothermic heat of reaction can reach 3450kw, temperature of reaction can be made to reach about 2680 DEG C, optimum operating condition 1300--1450 DEG C is being reacted for controlling working temperature in entrained-flow reactor, the nitrogen of required 3 ~ 5 times is reacted along reactor wall side direction spray people, in reactor, form eddy flow, shielding gas flow bed bioreactor 1, ensure the complete reaction of Si, SiC simultaneously; The Si of Reactive Synthesis
3n
4be deposited in reactor bottom water cooler, 600 ~ 800 DEG C are cooled to be transported in product feed bin 9 with the ratio of mixture of gas-solid mass ratio 1: 30 through product air conveyor 8 with pressurized air, the oxygen in pressurized air and SiC nitrogenize by-product carbon is utilized to react, the de-C of gasification, by ganging of products packing plant 10 metering packing, put in storage for sale; Reaction residue nitrogen carries the energy of 800--1000kw and a small amount of reaction product through pressure controller 2 with the temperature of 1300--1450 DEG C, regulates pressure-controlling flashboard 14 to regulate entrained-flow reactor internal pressure, enters in tunnel furnace 3, utilize high temperature N
2complete in tunnel furnace the nitrogenizing reaction sintering of the three-dimensional foam chemical stoneware filler prepared with SiC, Si binary sand be contained on kiln car 4, form silicon nitride combined silicon carbide three-dimensional foam chemical stoneware filler 16; The waste gas that tunnel furnace is discharged be temperature at the nitrogen of 300 ~ 600 DEG C, enter silica flour filtration cakes torrefaction machine 5 by pipeline, the dry silica flour filter cake from waste mortar treatment system, dried silica flour enters silica flour feed bin 6, and separating off nitrogen G&W vapor vent is discharged.
Nitrogen prepared by Nitrogen plant using air separation process 11 is the important factor that maintenance unit normally runs, carry and reactive material is provided, conveying reaction raw materials, derive heat of reaction, the multitasks such as dry reaction raw material, this unit adopts compression air separation device to produce nitrogen, market can be supplied by by-product high-purity oxygen, comprehensive power consumption is low, and under the commercioganic condition of oxygen, its comprehensive cost is lower than making nitrogen by pressure swing adsorption; Need Attended mode; Self-con-tained unit 12 is responsible for the production of whole production line, safe Automated condtrol and operation.
Claims (6)
1. prepare the unit of silicon nitride product with crystalline silicon processing waste mortar recovery silica flour, it is characterized in that: produce unit by entrained-flow reactor, nitrogen gas plasma lighter for ignition, pressure controller, tunnel furnace, kiln car, drying machine, silica flour feed bin, silica flour air conveyor, Si
3n
4air conveyor, Si
3n
4feed bin, ganging of products packing plant, Nitrogen plant using air separation process, robot control system(RCS) and relevant ducts, valve, instrument are formed; The synthesis of silicon nitride powder completes in the nucleus equipment-entrained-flow reactor of unit; Air flow bed operating pressure 0.2--1.6MPa, aspect ratio 3--10:1; The reaction sintering of silicon nitride combined silicon carbide stupalith completes in the key equipment-tunnel furnace of this unit; Tunnel furnace operating pressure≤0.1MPa, working sections amass be air flow bed sectional area 0.5--4 doubly, length be air flow bed height 5--20 doubly; Tunnel like sintered channels is combined to form with supporting kiln car; The silica flour reclaimed with crystalline silicon processing waste mortar and nitrogen, for raw material, take nitrogen as delivery vehicles, produce silicon nitride powder and silicon nitride combined silicon carbide stupalith.
2. crystalline silicon processing waste mortar according to claim 1 reclaims the unit that silicon nitride product prepared by silica flour, it is characterized in that: the raw material for the production of silicon nitride powder is the silicon powder utilizing crystalline silicon processing waste mortar to reclaim, its composition is Si>=80--95%, SiC≤20--5%, Fe
2o
3≤ 0.1%.
3. crystalline silicon processing waste mortar according to claim 1 reclaims the unit that silicon nitride product prepared by silica flour, it is characterized in that: the raw material for the production of silicon nitride powder is the nitrogen of purity 98--99.99%, output pressure 0.1--1.0MPa, the throughput of supporting nitrogen gas generating system is 2--8 times of actual nitrogenize consumption, to meet unit raw material and heat delivery needs.
4. crystalline silicon processing waste mortar according to claim 1 reclaims the unit that silicon nitride product prepared by silica flour, it is characterized in that: the raw material for the manufacture of silicon nitride combined silicon carbide stupalith is the binary sand that crystalline silicon processing waste mortar reclaims, and its composition is Si=40--20%, SiC=60--80%, Fe
2o
3≤ 0.1%.
5. crystalline silicon processing waste mortar according to claim 1 reclaims the unit that silicon nitride product prepared by silica flour, it is characterized in that: be that entrained-flow reactor is discharged for the production of the energy of silicon nitride combined silicon carbide stupalith sintering and nitrogen, reaction nitrogen that temperature 1200--1600 DEG C, pressure 0.01--0.10MPa contain a small amount of silicon nitride powder provides.
6. crystalline silicon processing waste mortar according to claim 1 reclaims the unit that silicon nitride product prepared by silica flour, it is characterized in that: the nitrogen transmitting device connecting entrained-flow reactor and tunnel furnace is pressure controller, its front end is provided with carries out pressure controlled automatically controlled valve according to entrained-flow reactor processing requirement, rear end is provided with the air distributor with tunnel kiln sintering process matching, pressure controller shell is metal shell, and liner can bear the lagging material of 1200--1600 DEG C.
Priority Applications (1)
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|---|---|---|---|
| CN201310024134.2A CN103183324B (en) | 2013-01-23 | 2013-01-23 | Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310024134.2A CN103183324B (en) | 2013-01-23 | 2013-01-23 | Unit for preparing silicon nitride product by silica powder recovered from crystalline silicon processed waste mortar |
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| CN103183324B true CN103183324B (en) | 2014-12-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539459A (en) * | 2013-09-28 | 2014-01-29 | 南昌大学 | Method for preparing alpha-phase-rich silicon nitride-silicon carbide composite powder from recycled silicon wafer fret saw dust powder |
| CN103553647B (en) * | 2013-10-08 | 2015-06-17 | 常州工程职业技术学院 | Method for preparation of silicon nitride bonded silicon carbide refractory material by using silicon cutting waste mortar |
| CN110423118B (en) * | 2019-07-24 | 2022-01-07 | 洛阳市科创绿色建材研究院 | Composite ceramic phase anti-seepage wear-resistant material for copper chute produced by polycrystalline silicon waste |
| CN113003549B (en) | 2021-03-08 | 2021-10-15 | 昆明理工大学 | Fast preparation of beta-Si by gas-solid reaction3N4And method thereof |
| CN113003551A (en) * | 2021-03-19 | 2021-06-22 | 尹克胜 | New technology for synthesizing aluminum nitride powder by melting and atomizing aluminum ingot and production unit thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351170C (en) * | 2005-12-07 | 2007-11-28 | 北京科技大学 | Process for ordinary pressure continuous synthesizing silicon nitride powder by fluidized bed tech. |
| CN200985280Y (en) * | 2006-12-07 | 2007-12-05 | 浙江大学 | Fluid-bed direct producing silicon nitride device |
| CN103058194B (en) * | 2008-09-16 | 2015-02-25 | 储晞 | Reactor for producing high-purity particulate silicon |
| CN102432296A (en) * | 2011-08-12 | 2012-05-02 | 尹克胜 | Comprehensive treatment technology of waste mortar in processing of photovoltaic crystalline silicon |
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