CN112999983A - Special atomizing synthetic furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingot - Google Patents
Special atomizing synthetic furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingot Download PDFInfo
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- CN112999983A CN112999983A CN202110317397.7A CN202110317397A CN112999983A CN 112999983 A CN112999983 A CN 112999983A CN 202110317397 A CN202110317397 A CN 202110317397A CN 112999983 A CN112999983 A CN 112999983A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 109
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 95
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 90
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000002844 melting Methods 0.000 title claims abstract description 24
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 24
- 230000008018 melting Effects 0.000 title claims abstract description 23
- 238000000889 atomisation Methods 0.000 claims abstract description 139
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 132
- 238000006243 chemical reaction Methods 0.000 claims abstract description 132
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 116
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 113
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 66
- 238000000034 method Methods 0.000 claims abstract description 40
- IWBUYGUPYWKAMK-UHFFFAOYSA-N [AlH3].[N] Chemical compound [AlH3].[N] IWBUYGUPYWKAMK-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000003595 mist Substances 0.000 claims abstract description 20
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 14
- 239000011819 refractory material Substances 0.000 claims abstract description 14
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003546 flue gas Substances 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 7
- 239000010959 steel Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 86
- 239000007788 liquid Substances 0.000 claims description 44
- 238000005121 nitriding Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 239000011449 brick Substances 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 239000006260 foam Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000010892 electric spark Methods 0.000 claims description 4
- 238000006722 reduction reaction Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 238000009827 uniform distribution Methods 0.000 claims description 4
- 238000004880 explosion Methods 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 239000012925 reference material Substances 0.000 claims description 3
- 229910017083 AlN Inorganic materials 0.000 claims 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims 2
- 239000004411 aluminium Substances 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 239000011810 insulating material Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 3
- 238000009688 liquid atomisation Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000011863 silicon-based powder Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- -1 aluminum silver Chemical compound 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
- B01J6/005—Fusing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0722—Preparation by direct nitridation of aluminium
- C01B21/0724—Preparation by direct nitridation of aluminium using a plasma
Abstract
The special atomizing synthesis furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots is similar to an acorn shape and comprises a pressure-bearing shell, a hearth inner cavity and a heat-insulating layer, wherein the pressure-bearing shell is an atomizing synthesis furnace shell, is made of boiler steel and is connected into a whole through a flange, a gasket and a fastening bolt; the inner cavity of the hearth is an atomization synthesis process reaction space, the upper seal head and the cylindrical atomization synthesis chamber are built by refractory materials resistant to high temperature of more than 1500 ℃, and the lower cone heat exchange chamber is built by refractory materials resistant to high temperature of more than 1200 ℃; a high-temperature resistant heat-insulating material is arranged between the hearth and the pressure-bearing shell; the atomization synthetic furnace is provided with an atomizer interface A, an igniter interface B, an observation sight glass E, a safety explosion-proof hole G, a high-temperature flue gas outlet C, a circulating nitrogen inlet D, a reaction product outlet F, a pressure measuring hole P, temperature measuring holes T1 and T2; the aluminum nitrogen cloud mist sprayed from the interface of the atomizer is ignited by an igniter to be atomized and synthesized into aluminum nitride micro powder, the aluminum nitride micro powder is discharged from a reaction product outlet after exchanging heat with circulating nitrogen, the temperature of the atomization synthesis chamber is controlled by adjusting the amount of the circulating nitrogen, and high-temperature flue gas is discharged from the top of the furnace.
Description
Technical Field
The invention relates to a special atomization synthesis furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots, belonging to the field of aluminum nitride powder material production equipment.
Background
Aluminum powder, also known as aluminum silver powder, CAS No: 7429-90-5 Risk markers: 10 (inflammable goods in wet), belonging to 1 dangerous goods of 4 categories, number 1309; the method is characterized in that the aluminum ingot is melted into aluminum liquid at about 850 ℃ in a melting furnace by taking natural gas combustion heat as a heat source, and the aluminum liquid is N at the temperature of 350-430 ℃ and the pressure of 3-8MPa2Under the action, the aluminum liquid is sprayed into fog shape by the atomizer, and a large amount of low-temperature nitrogen is used for rapidly absorbing the heat in the aluminum, so that the environmental temperature is lower than the nitriding reaction temperature of the aluminum, and the liquid aluminum in the shape of fog beads is rapidly condensed and contracted into a ball shape to prevent the aluminum powder from being nitrided; the solidified aluminum powder is separated into various particle size grades in a classifier; the nitrogen is reused after dust removal and purification; the atomization chamber is a process core device and is used for completing atomization of aluminum liquid into micro spherical fog drops, rapidly cooling and shaping, and preventing and eliminating nitridation of the atomized micro spherical aluminum powder as far as possible. The technological process of producing fine spherical aluminum powder with aluminum ingot fusion and atomization method belongs to the physical process.
The aluminum powder is a flammable and explosive dangerous article and has strict production, transportation and storage specifications and regulations, and aluminum ingots and aluminum liquid prepared by atomizing the aluminum powder are more stable and can be managed according to the management of common metal materials.
The aluminum nitride is a covalent bond compound, belongs to a hexagonal crystal system, has a lead-zinc ore type crystal structure, and is white or grey white. Molecular formula AlN, CAS No 24304-CrystalAnd is diamond-like nitride, and can be stabilized to 2200 ℃ at most. Strong room temperatureHigh in strength and slow in strength decrease with temperature increase.Thermal conductivityGood thermal expansion coefficient and is a good thermal shock resistant material. Resist againstMeltingMetalErosion ofHas strong capability, and is an ideal crucible material for casting pure iron, aluminum or aluminum alloy. Aluminum nitride is also an electrical insulator, has good dielectric properties, and is promising for use as an electrical component. The gallium arsenide surface has an aluminum nitride coating that protects it from ion implantation during annealing. The aluminum nitride is also hexagonalBoron nitrideConversion to cubic boron nitrideCatalyst and process for preparing same. Is a novel ceramic material with great development potential.
The production of aluminum nitride mainly comprises two methods, namely an aluminum oxide carbothermic reduction method and an aluminum powder direct nitriding synthesis method: the direct aluminum powder nitriding method is a well-established production method and is widely applied to the production of aluminum nitride, and the reaction equation 2Al + N2When the reaction is started at 500 ℃, the nitriding speed is obviously increased at 700 ℃, the aluminum powder surface is nitrided to generate an aluminum nitride layer in the initial stage of the reaction, and N is prevented2Or NH3Further diffusing to the center of aluminum powder particles, so that the yield of the prepared aluminum nitride is low; the reaction temperature is generally controlled to be 800-1200 ℃, the temperature exceeds the melting point of aluminum, and the aluminum powder and N2Or NH3A large amount of heat can be released in the reaction, in order to prevent the reaction from being over-temperature, a certain amount of aluminum nitride micro powder is added into the raw material aluminum powder to absorb the reaction heat and reduce the reaction temperature, so that the production efficiency is reduced, the danger and complexity of aluminum powder mixing in the material mixing process are increased, serious environmental pollution is caused, the aluminum nitride powder generated by the reaction is sintered and agglomerated, and the qualified aluminum nitride powder product can be obtained by complicated subsequent grinding processing.
The applicant combines two production technologies of aluminum ingot melting atomization superfine spherical aluminum powder and aluminum powder direct nitridation synthesis of aluminum nitride, simultaneously refers to the technologies of ZL201310024134.2 unit for preparing silicon nitride products by recycling silicon powder from crystalline silicon processing waste mortar and ZL201310024132.3 airflow bed reactor for preparing silicon nitride powder by recycling silicon powder from crystalline silicon processing waste mortar and the like which are previously developed by the applicant, and develops the technologies of eliminating aluminum powder transportation, storing, mixing aluminum nitride, heating and producingIn the intermediate links of product grinding and processing and the like, the aluminum nitride atomization synthesis furnace directly takes aluminum ingots as raw materials for melting and atomizing to synthesize aluminum nitride powder, and the materials not only have a physical process (aluminum liquid atomization) but also have violent chemical reaction (2Al + N)22AlN), N during the reaction2The gas changes into solid, the volume shrinks sharply, the pressure of the hearth is reduced, and nitrogen is needed to be supplemented to balance the pressure and temperature conditions of the hearth.
Disclosure of Invention
The invention aims to realize safe, stable, efficient and low-consumption production of aluminum nitride powder by directly synthesizing aluminum nitride micro powder in an atomization synthesis furnace from a molten aluminum ingot through redesigning an aluminum liquid atomization granulation chamber on the basis of a process technology for producing superfine spherical aluminum powder by melting and atomizing the aluminum ingot.
The purpose of the invention is realized as follows: the special atomizing synthesis furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots is similar to an acorn shape and comprises a pressure-bearing shell, a hearth inner cavity and a heat-insulating layer, wherein the pressure-bearing shell is an atomizing synthesis furnace shell, is made of an elliptical head and a boiler steel plate and is connected into a whole through a flange, a gasket and a fastening bolt; the inner cavity of the hearth is an atomization synthesis process reaction space, the upper seal head and the cylindrical atomization synthesis chamber are built by refractory materials capable of bearing high temperature of more than 1500 ℃, and the lower cone heat exchange chamber is built by refractory materials capable of bearing high temperature of more than 1200 ℃; a heat insulation layer is arranged between the refractory material masonry hearth and the pressure-bearing shell, and high-temperature-resistant foam brick masonry is filled; an atomizer interface A, an igniter interface B, an observation sight glass E, a safety explosion-proof hole G, a high-temperature flue gas outlet C, a circulating nitrogen inlet D, a reaction product outlet F, a pressure measuring hole P, temperature measuring holes T1 and T2 are arranged on the atomization synthesis furnace; the atomizing synthesis furnace works as follows: after various preparation works are done, an atomizer arranged on an atomization synthesis furnace interface A sprays aluminum liquid into a cylindrical synthesis chamber of the atomization synthesis furnace in a conical sector shape by taking compressed nitrogen as power to form aluminum nitrogen cloud mist capable of meeting aluminum nitriding conditions; starting an igniter arranged on an igniter interface B, igniting the aluminum nitrogen cloud mist, and triggering 2Al + N22AlN reaction, which is a strongly exothermic reaction, proceeds with the reactionThe furnace temperature rises rapidly, when the temperature of a temperature measuring point T1 on an end socket of the atomization synthesis furnace reaches 1000 ℃, the work of an igniter is stopped, the reaction is kept to be continuously carried out by means of reaction heat release, the atomized aluminum particles belong to high-activity particles, a layer of nano aluminum nitride film is easily formed on the surface of the particles in a low-temperature atomization environment, the further progress of the reaction is prevented, but the high-temperature environment can damage the layer of aluminum nitride film, the reaction is kept to be continuously carried out, the reason is that the thermal expansion coefficient of aluminum and aluminum nitride is not matched along with the mass increase of 51.85% and the volume expansion of 28.5% when aluminum is nitrified to form aluminum nitride, and Al is 25 x 10-6/kAlN＝4.6*10-6K, in the aluminum nitriding process, N2The gas is changed into solid, the volume is rapidly contracted to form a local negative pressure state around the particles, the peripheral nitrogen is rapidly supplemented to generate severe disturbance to the aluminum liquid particles, meanwhile, the aluminum liquid particles are rapidly heated and expanded to cause the aluminum nitride film wrapping the aluminum liquid particles to be damaged and expose the internal liquid level, the reaction is maintained to be continuously carried out, the aluminum nitride film on the surface of the aluminum liquid particles is continuously peeled off and suspended in the reaction atmosphere due to the severe changes of the volume and the quality of the raw materials and the products in the reaction process, and the aluminum nitride particles generated by the reaction are slowly settled in a hearth, enter a conical heat exchange chamber at the lower part and exchange heat with the circulating nitrogen input from a circulating nitrogen inlet D at the lower part of the heat exchange chamber because the reaction is carried out in an atomizing state and the distance between the particles is large and the particles are difficult to contact, collide and sinter into large particles, gradually cooling to below 150 ℃, and discharging the reaction product out of the atomization synthesis furnace from a reaction product outlet F at the bottom of the atomization synthesis furnace; circulating nitrogen enters the conical heat exchange chamber from an inlet D at the lower part of the heat exchange chamber in a tangent line, moves upwards in a rotational flow state, gradually increases the temperature in the heat exchange process with the settled aluminum nitride particles, lifts the settled particles, controls the settling speed of the settled particles, maintains the residence time of the particles in the furnace, ensures the complete nitridation of the Al particles, and ensures that the circulating nitrogen uniformly rises under the conditions of temperature rise and volume expansion in the heat exchange process by virtue of the conical heat exchange chamber, enters the atomization reaction chamber to participate in the reaction and regulates and controls the reaction temperature; the observation, adjustment and control of the whole working state of the atomization synthetic furnace are realized by observing the sight glass E and the safetyThe pressure gauge is arranged on the pressure measuring hole P of the end socket and is realized by temperature measuring and controlling instruments arranged at temperature measuring holes T1 and T2 in the middle parts of the end socket and the conical heat exchange chamber; 2Al + N2Al as a reference material, N is a strongly exothermic reaction of 2AlN2For controlling variables by pairing N2The control of the device can accurately control the reaction working conditions (including the temperature, the pressure, the residence time of solid particles and the like in the reaction zone of the atomizing synthesis furnace) of the atomizing synthesis furnace; n in and out of the atomized synthesis furnace2The method comprises the following steps of A, providing fresh nitrogen for a nitrogen preparation device, wherein the pressure is 0.5-10 MPa, the temperature is 300-700 ℃, the fresh nitrogen is used for atomizing aluminum liquid to form aluminum nitrogen cloud mist in an atomizing synthesis chamber, further nitriding the aluminum nitrogen cloud mist to synthesize silicon nitride, B, circulating nitrogen supplemented from the lower part of a heat exchange area of the atomizing synthesis chamber, the pressure is 3-500 kPa, the temperature is 30-100 ℃, the circulating nitrogen is used for exchanging heat with settled aluminum nitride particles, adjusting the temperature of the atomizing reaction chamber and participating in nitriding synthesis reaction, C, the high-temperature nitrogen leaves an end socket of the atomizing synthesis chamber, the pressure is 3-400 kPa, and the temperature is 1000-1500 ℃; n designed to maintain the nitridation reaction equilibrium2The modulus M is the ratio of A to 1.5-2M, B to 2-10M, C to A + B-M, and the yield of the product aluminum nitride to Al + M.
The pressure-bearing shell of the atomization synthetic furnace is made of a boiler steel plate and is connected into a whole through a flange, a gasket and a fastening bolt; the design pressure is 0.3-1.0MPa, the design temperature is 100 ℃, and the processing, manufacturing and acceptance are carried out according to GB/T150.1-150.4-2011 pressure vessel and TSG21-2016 fixed pressure vessel safety technology supervision regulations.
The inner cavity of the hearth of the atomization synthesis furnace is an atomization synthesis process reaction space, the upper seal head and the cylindrical atomization synthesis chamber are built by refractory materials capable of bearing high temperature of more than 1500 ℃, and the lower cone heat exchange chamber is built by refractory materials capable of bearing high temperature of more than 1200 ℃; and a heat insulation layer is arranged between the hearth built by refractory materials and the pressure-bearing shell, and high-temperature-resistant foam brick masonry is filled.
The atomizer interface A arranged on the atomization synthetic furnace is positioned in the middle of a cylindrical atomization reaction chamber of the atomization synthetic furnace, the interface is matched with an aluminum liquid atomizer joint, the interface is connected with a hearth inner cavity into a whole through a conical cavity, and a cavity masonry material is consistent with an atomization reaction chamber hearth material so as to meet the atomization condition of aluminum liquid, form aluminum-nitrogen mixed cloud mist with fine liquid drops and uniform distribution, and create conditions for continuous and uniform nitridation reaction.
The igniter interface B arranged on the atomization synthetic furnace and the atomizer interface A are arranged on the same plane and are arranged at 90 degrees with the atomizer interface A, and an igniter (the igniter has two forms of a nitrogen plasma igniter and an electric spark igniter) is connected and used for igniting and triggering the aluminum nitrogen cloud mist in the reaction chamber of the atomization synthetic furnace to generate 2Al + N2When 2AlN is reacted, aluminum nitride is produced.
The observation sight glass E arranged on the atomization synthetic furnace is symmetrically arranged with the atomizer interface A and is used for observing the working condition of the hearth of the atomization synthetic furnace.
The safe explosion-proof hole G arranged on the atomization synthetic furnace is symmetrically arranged with the igniter interface B, although 2Al + N2The 2AlN is a molecular reduction reaction, gas participating in the reaction becomes solid after the reaction, the volume is reduced, and the explosion danger is avoided, but considering that the reaction belongs to a strong exothermic reaction, a safety explosion-proof hole is required to be arranged, and the process safety of equipment is ensured.
The high-temperature flue gas outlet C arranged on the atomization synthesis furnace is positioned in the center of the seal head of the atomization synthesis furnace and used for discharging the flue gas (1300-1500 ℃ C. high-temperature nitrogen containing a small amount of aluminum nitride particles) of the atomization synthesis furnace.
The circulating nitrogen interface D arranged on the atomization synthetic furnace is positioned at the lower part of the conical heat exchange chamber of the atomization synthetic furnace and enters the hearth of the heat exchange chamber along a tangent line, so that circulating nitrogen forms a rotational flow to wash silicon nitride powder deposited on the inner wall of the heat exchange chamber, and the heat exchange efficiency of aluminum nitride particles settled from the upper part is improved.
The reaction product outlet F arranged on the atomization synthesis furnace is arranged at the lower end of the cone heat exchange chamber of the atomization synthesis furnace and is used for discharging aluminum nitride products produced by the atomization synthesis furnace.
The invention is further explained with reference to the figures and examples.
Drawings
FIG. 1 is a schematic diagram of an atomizing synthesizer.
FIG. 2 is an outline view of an atomized synthesizing furnace.
FIG. 3 is a top plan view of the top head of the atomizing synthesis furnace.
FIG. 4 is a cross-sectional view of a cylindrical atomization reaction chamber a-a of an atomization synthesis furnace.
FIG. 5 is a cross-sectional view of a conical heat exchange chamber b-b of the atomizing synthesizer.
FIG. 6 is a cross-sectional view of a conical heat exchange chamber c-c of the atomizing synthesizer.
The figures represent the structure of the atomizing synthesis furnace numerically: 1-a pressure-bearing shell of an atomization synthetic furnace, 2-a hearth cavity of the atomization synthetic furnace, 3-a heat-insulating layer between the pressure-bearing shell and the hearth cavity, wherein 1.1-a shell end enclosure, 1.2-a reaction chamber shell and 1.3-a heat exchange chamber conical shell; 2.1-seal head hearth masonry, 2.2-reaction chamber hearth masonry and 2.3-heat exchange chamber hearth masonry; 3.1-end enclosure heat-insulating layer, 3.2-reaction chamber heat-insulating layer, 3.3-heat exchange chamber heat-insulating layer,
the letters in the figure represent the process take-over numbers: a-an atomizer spray gun interface, B-an igniter interface, C-a high-temperature flue gas outlet, D-a circulating nitrogen inlet, E-an observation sight glass, an F-reaction product outlet, a G-safety explosion-proof hole, a P-pressure measuring hole and a T-temperature measuring hole.
The equipment mounting support can be modified and adjusted according to the mounting form and the field condition, and is not shown in the attached drawings.
Detailed Description
The following are specific examples of the present invention, but the method of the present invention is not limited thereto, and those skilled in the art can change or adjust the structure thereof as necessary.
Example 1:
FIGS. 1-6 show an atomizing synthetic furnace, wherein FIG. 1 shows the internal structure of the atomizing synthetic furnace, FIG. 2 shows the external view of the atomizing synthetic furnace, FIG. 3 shows the top head view of the top cover of the atomizing synthetic furnace, FIG. 4 shows the sectional view of the cylindrical atomizing reaction chamber a-a of the atomizing synthetic furnace, showing the structure and layout of various process connection pipes of the reaction chamber main body of the atomizing synthetic furnace, FIG. 5 shows the sectional view of the conical heat exchange chamber b-b of the atomizing synthetic furnace, showing the temperature measuring hole T2 of the conical heat exchange chamber of the atomizing synthetic furnace, FIG. 6 shows the sectional view of the conical heat exchange chamber c-c of the atomizing synthetic furnace, showing the structural layout of the circulating nitrogen inlet D of the conical heat exchange chamber of the atomizing synthetic furnace. The equipment mounting bracket not shown in the figure adopts an ear type bracket, and the adjustment is changed according to the mounting form and the field condition.
As shown in the figure: the special atomizing synthesis furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots is similar to an acorn shape and comprises a pressure-bearing shell 1, a hearth cavity 2 and a heat-insulating layer 3, wherein the pressure-bearing shell 1 of the atomizing synthesis furnace is made of boiler steel plates, the design pressure is 0.3MPa, the design temperature is 100 ℃, and the special atomizing synthesis furnace is processed, manufactured and accepted according to GB/T150.1-150.4-2011 pressure vessel and TSG21-2016 fixed pressure vessel safety technology supervision regulations. The shell end socket 1.1 is made of a standard elliptical end socket and a pressure container flange and is connected with the cylindrical atomization reaction chamber shell 1.2 and the conical heat exchange chamber shell 1.3 into a whole through flanges, gaskets and fastening bolts; the inner cavity of the hearth of the atomization synthesis furnace is an atomization synthesis process reaction space, an upper seal head 2.1 and a cylindrical atomization synthesis chamber 2.2 are built by white corundum refractory bricks, and a lower cone heat exchange chamber 2.3 is built by aluminum silicate refractory bricks; a heat insulation layer 3 is arranged between the firebrick masonry firebox and the pressure-bearing shell and is filled with high-temperature resistant foam brick masonry; an atomizer interface A arranged on the atomization synthesis furnace is positioned in the middle of a cylindrical atomization reaction chamber of the atomization synthesis furnace, the interface is matched with an aluminum liquid atomizer joint, a conical cavity is connected into a whole from the interface to the inner cavity of a hearth, and a cavity building material is consistent with the hearth material of the atomization reaction chamber so as to meet the atomization condition of aluminum liquid, form aluminum-nitrogen mixed cloud mist with fine liquid drops and uniform distribution, and create conditions for continuous and uniform nitridation reaction; an igniter interface B arranged on the atomization synthetic furnace and an atomizer interface A are arranged on the same plane and are 90 degrees to the atomizer interface A, and a nitrogen plasma igniter is connected for igniting and triggering the aluminum nitrogen cloud mist in the reaction chamber of the atomization synthetic furnace to generate 2Al + N2Reacting 2AlN to generate aluminum nitride; the observation sight glass E arranged on the atomization synthetic furnace is symmetrically arranged with the atomizer interface A and is used for observing the working condition of the hearth of the atomization synthetic furnace; the safe explosion-proof hole G arranged on the atomization synthetic furnace is symmetrically arranged with the igniter interface B, although 2Al + N22AlN is a molecular reduction reaction, and the gas participating in the reaction becomes solid after the reaction, so the volume is reduced, and the explosion danger does not exist, but the reaction is considered to be a strong exothermic reactionIt is necessary to provide a safety explosion-proof hole to ensure the process safety of the equipment; a high-temperature flue gas outlet C arranged on the atomization synthesis furnace is positioned in the center of a furnace top seal head of the atomization synthesis furnace and used for discharging flue gas (high-temperature nitrogen containing a small amount of aluminum nitride particles at 1300-1500 ℃) of the atomization synthesis furnace; a circulating nitrogen interface D arranged on the atomization synthesis furnace is positioned at the lower part of a conical heat exchange chamber of the atomization synthesis furnace and enters a hearth of the heat exchange chamber along a tangent line to enable circulating nitrogen to form a rotational flow so as to wash silicon nitride powder deposited on the inner wall of the heat exchange chamber and improve the heat exchange efficiency with aluminum nitride particles settled from the upper part, a reaction product outlet F arranged on the atomization synthesis furnace is arranged at the lower end of the conical heat exchange chamber of the atomization synthesis furnace and used for discharging aluminum nitride products produced by the atomization synthesis furnace, a seal head is provided with a pressure measuring hole P and a temperature measuring hole T1, and the middle part of the conical heat exchange chamber is provided with a temperature measuring hole T2 and used for detecting the working temperature and pressure inside the atomization; the atomizing synthesis furnace works as follows: starting a nitrogen plasma igniter arranged on an igniter interface B to form a nitrogen plasma environment in the furnace, starting an atomizer arranged on an atomizing and synthesizing furnace interface A, and spraying aluminum liquid into a cylindrical synthesizing chamber of the atomizing and synthesizing furnace in a conical sector shape by taking compressed nitrogen as power to form aluminum nitrogen cloud mist capable of meeting aluminum nitriding conditions; the aluminum nitrogen cloud is ignited by nitrogen plasma to trigger 2Al + N22AlN reaction, the furnace temperature rises rapidly, when the temperature of the temperature measuring point T1 on the end socket of the atomization synthesis furnace reaches 1000 ℃, the operation of the nitrogen plasma igniter is stopped, the reaction is kept to be continuously carried out by means of reaction heat release, the atomized aluminum particles belong to high-activity particles, a layer of nano aluminum nitride film is easily formed on the surfaces of the particles in a low-temperature atomization environment, the further progress of the reaction is prevented, but the high-temperature environment can damage the layer of aluminum nitride film, the reaction is kept to be continuously carried out, the reason is that the thermal expansion coefficients of aluminum and aluminum nitride are not matched along with 51.85 percent of mass increase and 28.5 percent of volume expansion when aluminum is nitrified to form the aluminum nitride, and Al is 25 x 10-6/k AlN＝4.6*10-6K, in the aluminum nitriding process, N2The gas is changed into solid, the volume is rapidly contracted to form a local negative pressure state around the particles, the peripheral nitrogen is rapidly supplemented to generate severe disturbance to the aluminum liquid particles, and simultaneously the aluminum liquid particles rapidly riseThe aluminum nitride film wrapping the aluminum liquid particles is damaged due to the expansion of temperature and volume, the liquid level in the aluminum liquid particles is exposed, the reaction is maintained to continue, the aluminum nitride film on the surface of the aluminum liquid particles is continuously peeled off and suspended in the reaction atmosphere because of the drastic change of the volume and the quality of raw materials and products in the reaction process, and the reaction is carried out in an atomization state, the distance between particles is large, the particles are difficult to contact, collide and sinter into large particles, the granularity of the aluminum nitride generated by the reaction is far smaller than the granularity of atomized aluminum drops, the aluminum nitride particles generated by the reaction are slowly settled in a hearth, enter a lower conical heat exchange chamber, exchange heat with circulating nitrogen input from a circulating nitrogen inlet D at the lower part of the heat exchange chamber, are gradually cooled to below 150 ℃, and are discharged out of the atomization synthesis furnace from a reaction product outlet F; circulating nitrogen enters the conical heat exchange chamber from an inlet D at the lower part of the heat exchange chamber in a tangent line, moves upwards in a rotational flow state, gradually increases the temperature in the heat exchange process with the settled aluminum nitride particles, lifts the settled particles, controls the settling speed of the settled particles, maintains the residence time of the particles in the furnace, ensures the complete nitridation of the Al particles, and ensures that the circulating nitrogen uniformly rises under the conditions of temperature rise and volume expansion in the heat exchange process by virtue of the conical heat exchange chamber, enters the atomization reaction chamber to participate in the reaction and regulates and controls the reaction temperature; the observation, adjustment and control of the whole working state of the atomization synthesis furnace are realized by an observation sight glass E, a pressure gauge arranged on a pressure measuring hole P of the seal head and temperature measuring and controlling instruments arranged at temperature measuring holes T1 and T2 in the middle of the seal head and the conical heat exchange chamber; 2Al + N2Al as a reference material, N is a strongly exothermic reaction of 2AlN2For controlling variables by pairing N2The control of the device can accurately control the reaction working conditions (including the temperature, the pressure, the particle residence time and the like of the reaction zone of the atomization synthesis furnace) of the atomization synthesis furnace; n in and out of the atomized synthesis furnace2The method comprises the following steps that A is fresh nitrogen provided by a nitrogen preparation device, the pressure is 0.5-10 MPa, the temperature is 300-700 ℃, the fresh nitrogen is used for atomizing aluminum liquid to form aluminum nitrogen cloud mist in an atomization synthesis chamber, and the aluminum nitrogen cloud mist is further nitrided to synthesize silicon nitride; b is circulating nitrogen supplemented from the lower part of a heat exchange area of the atomization synthesis furnace, the pressure is 3-500 kPa, the temperature is 30-100 ℃, and the circulating nitrogen is used for exchanging heat with the settled aluminum nitride particles, adjusting the temperature of the atomization reaction chamber and participating in nitrogenChemical synthesis reaction; c is high-temperature nitrogen leaving the seal head of the atomization synthesis furnace, the pressure is 3-400 kPa, and the temperature is 1000-1500 ℃; n designed to maintain the nitridation reaction equilibrium2The modulus M is the ratio of A to 1.5-2M, B to 2-10M, C to A + B-M, and the yield of the product aluminum nitride to Al + M.
Example 2:
FIGS. 1-6 show an atomizing synthetic furnace, wherein FIG. 1 shows the internal structure of the atomizing synthetic furnace, FIG. 2 shows the external view of the atomizing synthetic furnace, FIG. 3 shows the top head view of the top cover of the atomizing synthetic furnace, FIG. 4 shows the sectional view of the cylindrical atomizing reaction chamber a-a of the atomizing synthetic furnace, showing the structure and layout of various process connection pipes of the reaction chamber main body of the atomizing synthetic furnace, FIG. 5 shows the sectional view of the conical heat exchange chamber b-b of the atomizing synthetic furnace, showing the temperature measuring hole T2 of the conical heat exchange chamber of the atomizing synthetic furnace, FIG. 6 shows the sectional view of the conical heat exchange chamber c-c of the atomizing synthetic furnace, showing the structural layout of the circulating nitrogen inlet D of the conical heat exchange chamber of the atomizing synthetic furnace. The equipment mounting support not shown in the figure is modified and adjusted according to the mounting form and the field condition.
As shown in the figure: the special atomizing synthesis furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots is similar to an acorn shape and comprises a pressure-bearing shell 1, a hearth cavity 2 and a heat-insulating layer 3, wherein the pressure-bearing shell 1 of the atomizing synthesis furnace is made of a boiler steel plate, the design pressure is 0.8MPa, the design temperature is 150 ℃, and the special atomizing synthesis furnace is processed, manufactured and accepted according to GB/T150.1- -150.4- -2011 pressure vessel and TSG21-2016 fixed pressure vessel safety technology supervision regulations. The shell end socket 1.1 is made of an elliptical end socket and a flange and is connected with the cylindrical atomization reaction chamber shell 1.2 and the conical heat exchange chamber shell 1.3 into a whole through the flange, a gasket and a fastening bolt; the inner cavity of the hearth of the atomization synthesis furnace is an atomization synthesis process reaction space, an upper seal head 2.1 and a cylindrical atomization synthesis chamber 2.2 are built by silicon carbide refractory bricks, and a lower cone heat exchange chamber 2.3 is built by aluminum silicate refractory bricks; a heat insulation layer 3 is arranged between the firebrick masonry firebox and the pressure-bearing shell and is filled with high-temperature resistant foam brick masonry; the atomizer interface A arranged on the atomization synthetic furnace is positioned in the middle of the cylindrical atomization reaction chamber, the interface is matched with the aluminum liquid atomizer connector, and the interface is connected to the inner cavity of the hearthConical cavities are combined into a whole, and cavity building materials are consistent with the materials of a hearth of an atomization reaction chamber so as to meet the aluminum liquid atomization condition, form aluminum-nitrogen mixed cloud mist with fine liquid drops and uniform distribution, and create conditions for continuous and uniform nitridation reaction; the igniter interface B and the atomizer interface A are arranged on the same plane and are arranged at 90 degrees with the atomizer interface A, and the igniter is connected into an electric spark igniter to ignite and trigger the generation of 2Al + N by the aluminum nitrogen cloud fog in the reaction chamber of the atomization synthesis furnace22AlN reacts to generate aluminum nitride; the observation sight glass E is symmetrically arranged with the atomizer interface A to observe the working condition of the hearth of the atomized synthetic furnace; the safety explosion-proof hole G and the igniter interface B are symmetrically arranged to ensure the process safety of equipment; the high-temperature flue gas outlet C is positioned in the center of the seal head of the atomization synthesis furnace and used for discharging the flue gas (containing a small amount of aluminum nitride particles at the temperature of 1300-1500 ℃) of the atomization synthesis furnace; the circulating nitrogen interface D is positioned at the lower part of the conical heat exchange chamber of the atomizing synthetic furnace, and enters a hearth of the heat exchange chamber along a tangent line to enable circulating nitrogen to form rotational flow so as to wash silicon nitride powder deposited on the inner wall of the heat exchange chamber and improve the heat exchange efficiency with aluminum nitride particles settled from the upper part, a reaction product outlet F is arranged at the lower end of the conical heat exchange chamber of the atomizing synthetic furnace and is used for discharging aluminum nitride products produced by the atomizing synthetic furnace, a hearth end socket is provided with a pressure measuring hole P and a temperature measuring hole T1, and the middle part of the conical heat exchange chamber is provided with a temperature measuring hole T2 and is used for detecting the working temperature; the atomizing synthesis furnace works as follows: after various preparation works are done, an atomizer arranged on the interface A sprays aluminum liquid into a cylindrical synthesis chamber of the atomization synthesis furnace in a sector cone shape by taking compressed nitrogen as power to form aluminum nitrogen cloud mist meeting the aluminum nitriding condition; starting the electric spark igniter arranged on the interface B, igniting the aluminum nitrogen cloud mist, and triggering 2Al + N22AlN reaction, the furnace temperature rises rapidly along with the reaction, when the temperature of a temperature measuring point T1 on an end socket of the atomization synthesis furnace reaches 1000 ℃, the work of an igniter is stopped, the reaction is kept to be continuously carried out by the heat release of the reaction, the atomized aluminum particles belong to high-activity particles, a layer of nano aluminum nitride film is easily formed on the surfaces of the particles in a low-temperature atomization environment, the further progress of the reaction is prevented, but the high-temperature environment can damage the layer of aluminum nitride film, the reaction is kept to be continuously carried out, and the reason is that the aluminum nitride film can be damaged inFormation of aluminum nitride was accompanied by 51.85% mass gain and 28.5% volume expansion, the coefficient of thermal expansion of aluminum and aluminum nitride not matching, with Al 25 x 10-6/k AlN＝4.6*10-6The aluminum liquid particles are rapidly heated and expanded in volume in the aluminum nitriding process, aluminum nitride films wrapped by the aluminum liquid particles are broken through to expose the inner liquid level, the reaction is maintained to continue, the aluminum nitride films on the surfaces of the aluminum liquid particles are continuously peeled off and suspended in the reaction atmosphere due to the drastic change of the volume and the quality of raw materials and products in the reaction process, the reaction is carried out in an atomizing state, the distance between particles is large, the particles are difficult to contact, collide and sinter into large particles, the particle size of the aluminum nitride generated by the reaction is far smaller than the particle size of atomized aluminum droplets, the aluminum nitride particles generated by the reaction are slowly settled in a hearth, enter a lower conical heat exchange chamber, exchange heat with circulating nitrogen input from a circulating nitrogen inlet D at the lower part of the heat exchange chamber, are gradually cooled to below 150 ℃, and are discharged out of the atomizing synthesis furnace from a reaction product outlet F at; circulating nitrogen enters the conical heat exchange chamber from an inlet D at the lower part of the heat exchange chamber in a tangent line, moves upwards in a rotational flow state, gradually rises in temperature in the heat exchange process with settled aluminum nitride particles, lifts the settled particles, controls the settling speed of the settled particles, maintains the residence time of the particles in the furnace, ensures the complete nitridation of Al particles, solves the problem of uniform-speed rise of the circulating nitrogen under the conditions of temperature rise and volume expansion along with the heat exchange process by the conical heat exchange chamber, and enters the atomization reaction chamber to participate in the reaction and regulate and control the reaction temperature; the observation, adjustment and control of the whole working state of the atomization synthesis furnace are realized by an observation sight glass E, a pressure gauge arranged on a pressure measuring hole P of the seal head and temperature measuring and controlling instruments arranged at temperature measuring holes T1 and T2 in the middle of the seal head and the conical heat exchange chamber.
Claims (10)
1. A special atomizing synthetic furnace for synthesizing aluminum nitride powder by melting and atomizing aluminum ingots is characterized in that: the special atomizing synthesizing furnace for synthesizing aluminium nitride powder by melting and atomizing aluminium ingot is similar to acorn shape and is composed of pressure-bearing shell, hearth cavity and heat-insulating layer, the pressure-bearing shell is made up by using elliptical sealing head and boiler steel plate, and is connected with fastening bolt by means of flange, gasket and screwAre connected into a whole; the inner cavity of the hearth is an atomization synthesis process reaction space, the upper seal head and the cylindrical atomization synthesis chamber are built by refractory materials capable of bearing high temperature of more than 1500 ℃, and the lower cone heat exchange chamber is built by refractory materials capable of bearing high temperature of more than 1200 ℃; a heat insulation layer is arranged between the refractory material masonry hearth and the pressure-bearing shell, and high-temperature-resistant foam brick masonry is filled; an atomizer interface A, an igniter interface B, an observation sight glass E, a safety explosion-proof hole G, a high-temperature flue gas outlet C, a circulating nitrogen inlet D, a reaction product outlet F, a pressure measuring hole P, temperature measuring holes T1 and T2 are arranged on the atomization synthesis furnace; the atomizing synthesis furnace works as follows: after various preparation works are done, an atomizer arranged on an atomization synthesis furnace interface A sprays aluminum liquid into a cylindrical synthesis chamber of the atomization synthesis furnace in a conical sector shape by taking compressed nitrogen as power to form aluminum nitrogen cloud mist capable of meeting aluminum nitriding conditions; starting an igniter arranged on an igniter interface B, igniting the aluminum nitrogen cloud mist, and triggering 2Al + N22AlN reaction, the reaction is strong exothermic reaction, the furnace temperature rises rapidly along with the reaction, when the temperature of a temperature measuring point T1 on an end socket of the atomization synthesis furnace reaches 1000 ℃, the work of an igniter is stopped, the reaction is kept to be continuously carried out by the reaction exotherm, the atomized aluminum particles are high-activity particles, a layer of nano aluminum nitride film is easily formed on the surface of the particles under the low-temperature atomization environment, the reaction is prevented from further proceeding, but the high-temperature environment can damage the layer of aluminum nitride film, the reaction is kept to be continuously carried out, the reason is that the thermal expansion coefficient of aluminum and aluminum nitride is not matched along with 51.85 percent of mass increase and 28.5 percent of volume expansion when aluminum is nitrified to form aluminum nitride, and Al is 25 x 10-6/k AlN＝4.6*10-6K, in the aluminum nitriding process, N2The gas is changed into solid, the volume is rapidly contracted to form a local negative pressure state around the particles, the peripheral nitrogen is rapidly supplemented to generate severe disturbance to the aluminum liquid particles, meanwhile, the aluminum liquid particles are rapidly heated and expanded, so that an aluminum nitride film wrapping the aluminum liquid particles is damaged, the internal liquid level is exposed, the reaction is maintained to be continuously carried out, and the aluminum nitride film on the surface of the aluminum liquid particles is continuously peeled off and suspended in the reaction atmosphere due to the severe changes of the volume and the quality of the raw materials and the products in the reaction process, and the reaction is in an atomization stateThe particles are far away from each other, the particles are difficult to contact, collide and sinter into large particles, the particle size of aluminum nitride generated by reaction is far smaller than that of atomized aluminum drops, the aluminum nitride particles generated by reaction slowly settle in a hearth, enter a lower conical heat exchange chamber, exchange heat with circulating nitrogen input from a circulating nitrogen inlet D at the lower part of the heat exchange chamber, are gradually cooled to below 150 ℃, and are discharged out of an atomized synthetic furnace from a reaction product outlet F at the bottom of the atomized synthetic furnace; circulating nitrogen enters the conical heat exchange chamber from an inlet D at the lower part of the heat exchange chamber in a tangent line, moves upwards in a rotational flow state, gradually increases the temperature in the heat exchange process with the settled aluminum nitride particles, lifts the settled particles, controls the settling speed of the settled particles, maintains the residence time of the particles in the furnace, ensures the complete nitridation of the Al particles, and ensures that the circulating nitrogen uniformly rises under the conditions of temperature rise and volume expansion in the heat exchange process by virtue of the conical heat exchange chamber, enters the atomization reaction chamber to participate in the reaction and regulates and controls the reaction temperature; the observation, adjustment and control of the whole working state of the atomization synthesis furnace are realized by an observation sight glass E, a pressure gauge arranged on a pressure measuring hole P of the seal head and temperature measuring and controlling instruments arranged at temperature measuring holes T1 and T2 in the middle of the seal head and the conical heat exchange chamber; 2Al + N2Al as a reference material, N is a strongly exothermic reaction of 2AlN2For controlling variables by pairing N2The control of the device can accurately control the reaction working conditions (including the temperature, the pressure, the residence time of solid particles and the like in the reaction zone of the atomizing synthesis furnace) of the atomizing synthesis furnace; n in and out of the atomized synthesis furnace2The method comprises the following steps of A, providing fresh nitrogen for a nitrogen preparation device, wherein the pressure is 0.5-10 MPa, the temperature is 300-700 ℃, the fresh nitrogen is used for atomizing aluminum liquid to form aluminum nitrogen cloud mist in an atomizing synthesis chamber, further nitriding the aluminum nitrogen cloud mist to synthesize silicon nitride, B, circulating nitrogen supplemented from the lower part of a heat exchange area of the atomizing synthesis chamber, the pressure is 3-500 kPa, the temperature is 30-100 ℃, the circulating nitrogen is used for exchanging heat with settled aluminum nitride particles, adjusting the temperature of the atomizing reaction chamber and participating in nitriding synthesis reaction, C, the high-temperature nitrogen leaves an end socket of the atomizing synthesis chamber, the pressure is 3-400 kPa, and the temperature is 1000-1500 ℃; n designed to maintain the nitridation reaction equilibrium2The modulus M is the ratio of A to 1.5-2M, B to 2-10M, C to A + B-M, and the yield of the product aluminum nitride to Al + M.
2. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the pressure-bearing shell of the atomization synthetic furnace is made of a boiler steel plate and is connected into a whole through a flange, a gasket and a fastening bolt; the design pressure is 0.3-1.0MPa, the design temperature is 100 ℃, and the processing, manufacturing and acceptance are carried out according to GB/T150.1-150.4-2011 pressure vessel and TSG21-2016 fixed pressure vessel safety technology supervision regulations.
3. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the inner cavity of the hearth of the atomization synthesis furnace is an atomization synthesis process reaction space, the upper seal head and the cylindrical atomization synthesis chamber are built by refractory materials capable of bearing high temperature of more than 1500 ℃, and the lower cone heat exchange chamber is built by refractory materials capable of bearing high temperature of more than 1200 ℃; and a heat insulation layer is arranged between the hearth built by refractory materials and the pressure-bearing shell, and high-temperature-resistant foam brick masonry is filled.
4. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the atomizer interface A arranged on the atomization synthetic furnace is positioned in the middle of a cylindrical atomization reaction chamber of the atomization synthetic furnace, the interface is matched with an aluminum liquid atomizer joint, the interface is connected with a hearth inner cavity into a whole through a conical cavity, and a cavity masonry material is consistent with an atomization reaction chamber hearth material so as to meet the atomization condition of aluminum liquid, form aluminum-nitrogen mixed cloud mist with fine liquid drops and uniform distribution, and create conditions for continuous and uniform nitridation reaction.
5. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the igniter interface B arranged on the atomization synthetic furnace and the atomizer interface A are arranged on the same plane at 90 degrees, and an igniter (the igniter has two forms of a nitrogen plasma igniter and an electric spark igniter) is connected and used for igniting and triggering aluminum nitrogen in a reaction chamber of the atomization synthetic furnaceCloud generation of 2Al + N2When 2AlN is reacted, aluminum nitride is produced.
6. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the observation sight glass E arranged on the atomization synthetic furnace is symmetrically arranged with the atomizer interface A and is used for observing the working condition of the hearth of the atomization synthetic furnace.
7. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the safe explosion-proof hole G arranged on the atomization synthetic furnace is symmetrically arranged with the igniter interface B, although 2Al + N2The 2AlN is a molecular reduction reaction, nitrogen participating in the reaction becomes solid after the reaction, the volume is reduced, and the explosion danger is avoided, but considering that the reaction belongs to a strong exothermic reaction, a safety explosion-proof hole is required to be arranged, and the process safety of equipment is ensured.
8. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the high-temperature flue gas outlet C arranged on the atomization synthesis furnace is positioned in the center of the seal head of the atomization synthesis furnace and used for discharging the flue gas (1300-1500 ℃ C. high-temperature nitrogen containing a small amount of aluminum nitride particles) of the atomization synthesis furnace.
9. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the circulating nitrogen interface D arranged on the atomization synthetic furnace is positioned at the lower part of the conical heat exchange chamber of the atomization synthetic furnace and enters the hearth of the heat exchange chamber along a tangent line, so that circulating nitrogen forms a rotational flow to wash silicon nitride powder deposited on the inner wall of the heat exchange chamber, and the heat exchange efficiency of aluminum nitride particles settled from the upper part is improved.
10. The special atomization synthesis furnace for synthesizing the aluminum nitride powder by melting and atomizing the aluminum ingot according to claim 1, characterized in that: the reaction product outlet F arranged on the atomization synthesis furnace is arranged at the lower end of the cone heat exchange chamber of the atomization synthesis furnace and is used for discharging aluminum nitride products produced by the atomization synthesis furnace.
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| CN113457577A (en) * | 2021-07-06 | 2021-10-01 | 淄博胜赢化工有限公司 | Raw material mixing and melting device for producing p-tert-butyl catechol and use method thereof |
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