CN110182772B - Method for synthesizing aluminum nitride by rotary kiln method - Google Patents
Method for synthesizing aluminum nitride by rotary kiln method Download PDFInfo
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- CN110182772B CN110182772B CN201910496105.3A CN201910496105A CN110182772B CN 110182772 B CN110182772 B CN 110182772B CN 201910496105 A CN201910496105 A CN 201910496105A CN 110182772 B CN110182772 B CN 110182772B
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- rotary kiln
- nitrogen
- aluminum nitride
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- 238000000034 method Methods 0.000 title claims abstract description 41
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 26
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 abstract description 18
- 238000003786 synthesis reaction Methods 0.000 abstract description 17
- 230000015572 biosynthetic process Effects 0.000 abstract description 15
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000498 cooling water Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000446 fuel Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910001337 iron nitride Inorganic materials 0.000 description 1
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Muffle Furnaces And Rotary Kilns (AREA)
Abstract
The invention discloses a method for synthesizing aluminum nitride by a rotary kiln method, which comprises the following steps: spraying aluminum powder from a solid powder feeding port on the rotary kiln body; introducing nitrogen from a nitrogen inlet on the rotary kiln main body; the nitrogen and the aluminum powder carry out self-propagating reaction in the rotary kiln body to generate nitride. The method for synthesizing the aluminum nitride by the rotary kiln method can realize the mass continuous synthesis of the aluminum nitride.
Description
Technical Field
The invention relates to the field of nitride synthesis, and further relates to a method for synthesizing aluminum nitride by a rotary kiln method.
Background
Nitrides, especially aluminum nitride, are widely used industrially. Such as aluminum nitride, can be used to make high temperature resistant components, heat transfer components, and the like.
The self-propagating technology is a method of synthesizing a material by using self-heat emission of a chemical reaction, and is favored in the industry because the reaction can be continued by self-heat emission of the chemical reaction and can be continued without an external heat source.
The rotary kiln is used as a nitride synthesis reactor, and reactants are continuously fed into the furnace, the synthesis reaction is continuously carried out, and products are continuously discharged from the furnace in a micro-positive pressure state. Is a high-efficiency energy-saving synthesis device.
The existing nitride synthesis reactor is mainly a closed reactor. Some require high pressure (such as high pressure self-propagating processes); some require heating and consume high energy (such as vacuum resistance furnace method). The existing method is an intermittent production method, has low production efficiency, and needs integral equipment and process improvement urgently.
Disclosure of Invention
Technical problem to be solved
In view of the above, the present invention aims to provide a method for synthesizing aluminum nitride by a rotary kiln method, which at least partially solves the above problems.
(II) technical scheme
In order to achieve the above object, the present invention provides a method for synthesizing aluminum nitride by a rotary kiln method, which comprises:
spraying aluminum powder from a solid powder feeding port on the rotary kiln body;
introducing nitrogen from a nitrogen inlet on the rotary kiln main body;
and the nitrogen and the aluminum powder perform self-propagating reaction in the rotary kiln body to generate aluminum nitride.
In a further embodiment, further comprising: before spraying aluminum powder and nitrogen into the rotary kiln main body, the interior of the rotary kiln main body is heated to a set temperature by using combustible gas, and the moisture and oxygen in the interior are removed.
In a further embodiment the aluminium powder is injected into the body of the rotary kiln at a mass flow rate of 1 to 1000 kg/h.
In a further embodiment, the nitrogen is introduced into the rotary kiln body at a flow rate of 1 to 830Nm3/h。
In a further embodiment, the aluminum powder has a particle size of 0.1 μm to 10 μm.
In a further embodiment, the rotary kiln is maintained at a slightly positive pressure atmosphere of from 100Pa to 1000Pa while the self-propagating reaction is carried out.
In a further embodiment, the method also comprises the step of cooling the aluminum nitride output from the rotary kiln body by circulating water through a cooling system.
(III) advantageous effects
The aluminum nitride is prepared by a rotary kiln method, so that a large amount of continuous synthesis of the aluminum nitride can be realized;
according to the invention, materials are fed at a material inlet in a pulse pneumatic mode at a set flow rate, so that the material distribution is uniform, the powder supply speed is adjustable, and no dust is leaked;
the method adopts a micro-positive pressure self-propagating reaction method, and heating is not needed during the reaction, so that energy can be saved.
The method disclosed by the invention has a particularly remarkable effect on preparing the aluminum nitride, and can realize the preparation of the aluminum nitride with high efficiency, high quality and low energy consumption.
Drawings
FIG. 1 is a flow chart of a rotary kiln method for synthesizing aluminum nitride according to an embodiment of the present invention.
FIG. 2 is a schematic diagram of a rotary kiln nitride self-propagating synthesis apparatus according to an embodiment of the present invention.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments. In the specification, the same or similar reference numerals denote the same or similar components. The following description of the embodiments of the present invention with reference to the accompanying drawings is intended to explain the general inventive concept of the present invention and should not be construed as limiting the invention.
Throughout the specification, reference to "one embodiment," "an embodiment," "one example," or "an example" means: the particular features, structures, or characteristics described in connection with the embodiment or example are included in at least one embodiment of the invention. Thus, the appearances of the phrases "in one embodiment," "in an embodiment," "one example" or "an example" in various places throughout this specification are not necessarily all referring to the same embodiment or example. Furthermore, the particular features, structures, or characteristics may be combined in any suitable combination and/or sub-combination in one or more embodiments or examples. Further, as used herein, the term "and/or" will be understood by those of ordinary skill in the art to include any and all combinations of one or more of the associated listed items.
First, an electrical apparatus for implementing the method for synthesizing aluminum nitride by the rotary kiln method according to the embodiment of the present invention is introduced, and fig. 2 is a schematic view of a nitride self-propagating synthesis apparatus by the rotary kiln method according to the embodiment of the present invention. The embodiment of the invention provides a rotary kiln method nitride self-propagating synthesis device which comprises a rotary kiln main body 1, a solid powder feeding port 2 and a nitrogen inlet 3. The rotary kiln body 1 is disposed obliquely and configured to be driven to rotate. The solid powder feeding port 2 is arranged at the higher end of the rotary kiln body which is obliquely arranged and used for inputting solid powder; the nitrogen inlet 3 is used for introducing nitrogen into the rotary kiln main body and providing a conveying gas source for the pulse pneumatic assembly, the pulse pneumatic assembly 21 is arranged on the solid powder feeding port 2 and used for spraying reaction solid powder into the rotary kiln main body 1, and through the arrangement, nitrogen and the solid powder generate self-propagating reaction in the rotary kiln to generate nitride. The rotary kiln provided by the embodiment of the invention works in a micro-positive pressure state (100Pa-1000Pa), reactants participating in the reaction continuously enter the furnace, the self-propagating synthesis reaction is continuously carried out, and products are continuously discharged from the furnace.
The rotary kiln body 1 of the synthesis equipment is of a cylindrical structure, and is inclined at a certain angle with the ground, wherein the inclination angle is greater than 0 degrees and less than 90 degrees, and further, the preferable inclination angle is greater than 0 degrees and less than or equal to 10 degrees. Two rolling rings, namely a first rolling ring 11 and a second rolling ring 12 are arranged at proper points of the inclined rotary kiln body 1, and the two rolling rings are located on the supporting riding wheels. When the rotary kiln rotates, one supporting wheel 61 rotates in the same direction as the rotary kiln, and the other supporting wheel 62 rotates in the opposite direction. In the embodiment, the rotary kiln main body 1 can be made of steel plate structure on the outside and a fireproof, heat-preservation and heat-insulation layer is built inside. Since the self-propagating reaction does not need to be heated additionally, the non-reaction area of the rotary kiln body 1 can be constructed by designing and selecting refractory materials with lower refractoriness. The nitrides produced by the reaction in the rotary kiln body 1 gradually move in the axial direction of the rotary kiln towards the lower end of the rotary kiln. The rotary kiln body 1 in the embodiment is configured to be driven to rotate, the rotation of the rotary kiln is realized by driving of the motor 7, and the rotation speed of the rotary kiln can be adjusted by adopting an automatic speed regulating system. To achieve efficient, continuous production of nitrides, the preferred length of the rotary kiln body 1 is between 1 and 40 meters.
In one embodiment, a refractory heat-insulating layer is built on the inner wall of the rotary kiln body 1 corresponding to the reaction zone to protect the shell of the barrel body and ensure that the reaction zone has enough temperature.
The solid powder feeding port 2 is arranged at the higher end of the rotary kiln main body 1 to guide solid materials into the rotary kiln main body 1; the nitrogen inlet 3 is arranged at the higher end of the furnace body and is configured to form a self-propagating reaction with the solid powder in the rotary kiln body 1 after nitrogen is introduced, and simultaneously provide an air source for powder conveying. The discharge port 4 is opened at a lower end (i.e., the bottom of the furnace body) of the rotary kiln body 1, and is configured to output the nitride after the self-propagating reaction.
The solid powder inlet 2 of the synthesis equipment is a feed inlet for qualified reactant powders, which can be prepared in advance. The particle size of the powder should be as small as possible to allow self-propagating reactions. The particle size of the self-propagating reaction is generally 0.1 μm to 100. mu.m. The prior art does not have a process for preparing aluminum nitride, silicon nitride and silicon iron nitride by adopting a rotary kiln self-propagating mode, and the nitride can be prepared in a large amount, continuously, efficiently and energy-saving manner by adopting the rotary kiln self-propagating mode.
In one embodiment, the solid powder inlet 2 of the synthesis apparatus is provided with a pulsed pneumatic assembly 21. As nitrogen is required to be introduced as reaction gas during the self-propagating reaction in the rotary kiln body 1, a certain pressure is required in a hearth, and a pressure difference exists between the inside and the outside. And a pulse pneumatic assembly 21 is arranged on the solid powder feeding port 2, and reaction powder is sprayed into the furnace. The pulse pneumatic assembly 21 can control the injection amount of the solid powder.
The nitrogen inlet 3 of the synthesis apparatus is used for introducing the reaction gas, and the nitrogen-containing gas introduced into the reaction in this embodiment is preferably nitrogen. In one embodiment, a valve and flow meter 31 may be provided at the nitrogen inlet 3 for controlling the gas flow. In one embodiment, the nitrogen inlet 3 may be opened at the upper end of the rotary kiln body 1 where mixing with the solid powder begins. Nitrogen gas introduced from an inlet 3 fills the rotary kiln body 1, and a slight positive pressure atmosphere (100Pa to 1000Pa) is maintained therein.
In one embodiment, the synthesis equipment can be further provided with a movable fuel nozzle, in order to ensure the initial condition of the self-propagating reaction, in the pretreatment stage, flame can be generated through the fuel nozzle to heat the interior of the furnace body, the rotary kiln body can be heated to the temperature capable of carrying out the self-propagating reaction through heating, water vapor, oxygen and the like in the furnace body are removed in the heating process, and external heating equipment and vacuumizing equipment are not needed during normal production.
In one embodiment, the discharge port 4 of the rotary kiln body 1 is followed by a cooling system to forcibly cool the reaction product. The cooling system can comprise a bottom cooling system discharge port 53, a cooling water inlet 51 and a cooling water outlet 52, a cooling pipeline arranged in a surrounding mode is connected between the cooling water inlet 51 and the cooling water outlet 52, a cooling medium (such as water) is introduced from the cooling water inlet 51, and flows out from the cooling water outlet 52 after being circulated, the temperature of nitride in the cooling system can be gradually reduced in the process, and the nitride can be discharged from the cooling system discharge port 4 after the temperature of the nitride material is reduced to a set temperature.
FIG. 1 is a flow chart of a rotary kiln method for synthesizing aluminum nitride according to an embodiment of the present invention. As shown in fig. 1, the method for preparing aluminum nitride by the above synthesis apparatus may include the steps of:
s101: spraying aluminum powder from a solid powder feeding port on the rotary kiln body;
s102: introducing nitrogen from a nitrogen inlet on the rotary kiln main body;
s103: and the nitrogen and the aluminum powder perform self-propagating reaction in the rotary kiln body to generate aluminum nitride.
In some embodiments, the blow-in process is, before step S101, igniting a fuel nozzle, heating the inside of the furnace body through the ignited fuel nozzle, dehydrating the inside of the furnace body, heating to a temperature at which the self-propagating reaction can proceed, and consuming oxygen located in the furnace body through the process, ensuring a nitrogen atmosphere for the self-propagating reaction, which is summarized as dry heat accumulation.
In the step S101, solid powder with a particle size smaller than a set particle size needs to be selected to participate in the reaction so as to ensure that the self-propagating reaction is continuously carried out, wherein the selectable particle size is 0.1-10 microns; meanwhile, the aluminum powder can be sprayed from a solid material inlet in a pulse pneumatic mode, the input solid reactant flow can be ensured, and the optional mass flow is 1-1000 kg/h.
In step S102, the self-propagating reaction is usually a reaction between a gas and a solid, and a reaction gas is also introduced when the aluminum powder is injected, wherein the reaction gas is nitrogen gas based on the requirement of the product (nitride). Optionally, the flow rate of the introduced nitrogen is 1-830Nm3The temperature of the introduced nitrogen is normal temperature.
In step S103, the self-propagating reaction continues to proceed under the condition that the self-propagating reaction is satisfied, and nitrides continue to be generated in the furnace.
In one embodiment, when the reaction product is aluminum nitride, the solid powder introduced into the rotary kiln body is aluminum powder, the particle size is preferably several micrometers (0.1 μm to 10 μm), and the mass flow rate of the introduced powder is 1 to 1000 kg/h.
Further, it should be noted that the above steps S1-S3 are only used to distinguish the reaction steps, and the sequence of some steps may be different or may be performed simultaneously, for example, the steps S1 and S2 may be performed simultaneously.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for synthesizing aluminum nitride by a rotary kiln method comprises the following steps:
spraying aluminum powder from a solid powder feeding port on the rotary kiln body;
introducing nitrogen from a nitrogen inlet on the rotary kiln main body;
the nitrogen and the aluminum powder perform self-propagating reaction in the rotary kiln main body to generate aluminum nitride;
and the rotary kiln keeps a micro-positive pressure atmosphere of 100Pa-1000Pa when the self-propagating reaction is carried out.
2. The method as claimed in claim 1, wherein the inside of the rotary kiln body is heated to a set temperature with combustible gas before injecting the aluminum powder and the nitrogen gas into the rotary kiln body, and moisture and oxygen are removed from the inside.
3. The method as claimed in claim 1, wherein the aluminum powder is injected into the body of the rotary kiln at a mass flow rate of 1 to 1000 kg/h.
4. A method as claimed in claim 1, wherein the nitrogen is passed into the body of the rotary kiln at a flow rate of from 1 to 830Nm3/h。
5. The method of claim 1, wherein the aluminum powder has a particle size of 0.1-10 μm.
6. The method of claim 1, further comprising cooling the aluminum nitride output from the rotary kiln body with circulating water via a cooling system.
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| CN201910496105.3A CN110182772B (en) | 2019-06-10 | 2019-06-10 | Method for synthesizing aluminum nitride by rotary kiln method |
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| CN201910496105.3A CN110182772B (en) | 2019-06-10 | 2019-06-10 | Method for synthesizing aluminum nitride by rotary kiln method |
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| CN110182772B true CN110182772B (en) | 2020-04-21 |
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| DE69204996T2 (en) * | 1991-03-22 | 1996-02-08 | The Dow Chemical Co., Midland, Mich. | METHOD FOR CARBOTHERMAL PRODUCTION OF NON-OXIDE CERAMIC POWDER IN A HIKING BED. |
| CN1191194C (en) * | 2003-06-04 | 2005-03-02 | 北京科技大学 | Method for preparing aluminium nitrides and nitrogen oxides by combustion synthesis |
| US7011804B2 (en) * | 2003-07-02 | 2006-03-14 | Taiwan Salt Company | Method and apparatus for preparing aluminum nitride |
| CN109020555A (en) * | 2018-09-14 | 2018-12-18 | 青岛瓷兴新材料有限公司 | A method of the conbustion synthesis aluminium nitride powder under micro-positive pressure flowing nitrogen atmosphere |
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Denomination of invention: Method for synthesizing aluminum nitride by rotary kiln method Effective date of registration: 20240102 Granted publication date: 20200421 Pledgee: Ningxia East Guarantee Co.,Ltd. Pledgor: Ningxia Shixing Technology Co.,Ltd. Registration number: Y2023640000053 |
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