CN107804830A - The preparation method of titanium nitride - Google Patents
The preparation method of titanium nitride Download PDFInfo
- Publication number
- CN107804830A CN107804830A CN201711206023.8A CN201711206023A CN107804830A CN 107804830 A CN107804830 A CN 107804830A CN 201711206023 A CN201711206023 A CN 201711206023A CN 107804830 A CN107804830 A CN 107804830A
- Authority
- CN
- China
- Prior art keywords
- titanium nitride
- preparation
- titanium
- valve
- nitrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01B21/076—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 titanium or zirconium or hafnium
- C01B21/0761—Preparation by direct nitridation of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to the preparation method of titanium nitride, belong to smelting field of nonferrous metal.The technical problems to be solved by the invention are to provide the preparation method of titanium nitride, and for this method using titanium valve as raw material, nitrogen or ammonia are source of the gas, are nitrogenized using fluid bed, produce titanium nitride.The preparation method of titanium nitride of the present invention mainly has advantages below：1st, gained titanium nitride purity is very high, can stably reach 99.9%；2nd, the particle diameter of product is small and is evenly distributed, and titanium nitride powder of the granularity in below 50um can be prepared；3rd, can be produced under as little as 800 DEG C of temperature conditionss, it is less demanding to reaction condition, greatly reduce energy consumption；4th, by adjusting nitridation time, air inflow and input and output material time, the continuous production of titanium nitride can be realized.
Description
Technical field
The present invention relates to the preparation method of titanium nitride, belong to smelting field of nonferrous metal.
Background technology
Titanium nitride is a kind of new function material, has high golden yellow metallic luster, hardness, fusing point height, chemical property steady
Fixed, good conductivity, with metal material mutually excellent chemical and physical properties such as molten.So far, titanium nitride has been applied to height
The fields such as level refractory material, special type knife, flawless finish material, high-temperature electric conduction material and the lining material of metal surface, together
When, also it is applied to ferrous materials as reinforcing agent, there is vast potential for future development.
At present, industrially preparing the method for titanium nitride mainly includes titanium valve nitridation working system and TiO2Carbon thermal reduction produces
Method.Wherein, titanium valve nitridation working system easily sinters, and causes the particle diameter of gained titanium nitride larger and uneven；Using TiO2
Carbon thermal reduction working system, temperature, which will at least reach 1300 DEG C, can just produce titanium nitride, and need to improve constantly temperature and can just make
Reaction is thorough, moreover, obtained titanium nitride powder generally contains higher oxygen content, oxygen is titanium nitride usual impurities, causes to produce
Product purity reduces, therefore generally also needs to carry out purified treatment to product.Drawbacks described above present in existing production method is significantly
Limit the further genralrlization application of titanium nitride.
Therefore, need badly and provide that a kind of cost is relatively low, nitridation not harsh to working condition requirement and suitable large-scale production
The preparation method of titanium.
The content of the invention
It is an object of the invention to provide the preparation method of titanium nitride.
The invention provides the preparation method of titanium nitride, and using titanium valve as raw material, nitrogen or ammonia are source of the gas, using fluid bed
Nitridation, produces titanium nitride.
Further, the particle diameter of the titanium valve is below 45 μm.
Further, the air velocity of the source of the gas is 2.5~3.5m/s.
Further, the nitriding temperature is 800~1200 DEG C.
Further, the nitridation time is 1~4h.
Further, described preparation method comprises the following steps：Fluidized furnace is heated, controls the throughput of source of the gas, is added
Titanium valve, titanium valve are suspended on fluid bed, are reacted with nitrogen, are produced titanium nitride.
Further, described preparation method also comprises the following steps：
A, titanium nitride is collected：Air velocity is adjusted to more than 0.02m/s, the titanium nitride of generation is blown in collector, when
Between be 5~10min, collect titanium nitride；
B, continuous production：Air velocity is adjusted to 0.003~0.02m/s, titanium valve is added and continues to nitrogenize.
Further, the time that titanium nitride is blown to collector by step a is 5~10min.
The invention provides the preparation method of titanium nitride, this method mainly has advantages below：1st, gained titanium nitride purity
It is very high, 99.9% can be stably reached；2nd, the particle diameter of product is small and is evenly distributed, and granularity can be prepared below 50um's
Titanium nitride powder；3rd, can be produced under as little as 800 DEG C of temperature conditionss, it is less demanding to reaction condition, greatly reduce
Energy consumption；4th, by adjusting nitridation time, air inflow and input and output material time, the continuous production of titanium nitride can be realized.
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
The invention provides the preparation method of titanium nitride, using titanium valve as raw material, with reference to fluidization technology Direct-Nitridation, you can
Titanium nitride powder is prepared.At present, there is not yet producing the relevant report of titanium nitride by fluid bed.
Illustrated below, the present invention is by rationally controlling titanium valve powder size, stream of nitrogen gas amount, nitridation time, nitridation
The technological parameters such as temperature, the titanium nitride powder of high pure and ultra-fine can be prepared.
Embodiment 1 prepares titanium nitride using the inventive method
Using 45um titanium valves as raw material, nitrogen is source of the gas.
Fluidized furnace is heated to 1200 DEG C, while it is 3m/s to control stream of nitrogen gas speed, and titanium valve, titanium valve are added from charge door
It is suspended on fluid bed.Titanium valve reacts with nitrogen, generates titanium nitride, and titanium nitride is also suspended in fluid bed, nitridation time 2h, titanium valve
With nitrogen all with reference to generation titanium nitride.
Increase air velocity to blow to titanium nitride is generated in collector to 6m/s, the time is about 5~10 minutes.Then by nitrogen
Gas air velocity is adjusted to 3m/s, adds titanium valve and continues to nitrogenize, realizes continuous production.
After collector temperature is down to normal temperature, collector is opened, takes out product, sample presentation detection is carried out to the product, granularity is sieved
Point.Its chemistry is into predominantly Ti, N, and Ti and N content is 99.9% in product, powder size 45um~50um.
Embodiment 2 prepares titanium nitride using the inventive method
Using 30um titanium valves as raw material, nitrogen is source of the gas.
Fluidized furnace is heated to 1000 DEG C, while it is 3.5m/s to control stream of nitrogen gas speed, and titanium valve, titanium are added from charge door
Powder is suspended on fluid bed.Titanium valve reacts with nitrogen, generates titanium nitride, and titanium nitride is also suspended in fluid bed, nitridation time 4h, titanium
Powder is with nitrogen all with reference to generation titanium nitride.
Increase air velocity to blow to titanium nitride is generated in collector to 3m/s, the time is about 5~10 minutes.Then by nitrogen
Gas air velocity is adjusted to 6m/s, adds titanium valve and continues to nitrogenize, realizes continuous production.
After collector temperature is down to normal temperature, collector is opened, takes out product, sample presentation detection is carried out to the product, granularity is sieved
Point.Its chemistry is into predominantly Ti, N, and Ti and N content is 99.9% in product, granularity 30um~35um.
Claims (8)
1. the preparation method of titanium nitride, it is characterized in that：Using titanium valve as raw material, nitrogen or ammonia are source of the gas, are nitrogenized using fluid bed,
Produce titanium nitride.
2. preparation method as claimed in claim 1, it is characterized in that：The particle diameter of the titanium valve is below 45 μm.
3. preparation method as claimed in claim 1, it is characterized in that：The air velocity of the source of the gas is 2.5~3.5m/s.
4. preparation method as claimed in claim 1, it is characterized in that：The nitriding temperature is 800~1200 DEG C.
5. the preparation method as described in claim 1 or 4, it is characterized in that：The nitridation time is 1~4h.
6. preparation method as claimed in any one of claims 1 to 5, wherein, it is characterized in that：Comprise the following steps：Heat fluidized furnace,
The throughput of source of the gas is controlled, adds titanium valve, titanium valve is suspended on fluid bed, is reacted with nitrogen, is produced titanium nitride.
7. preparation method as claimed in claim 6, it is characterized in that：Also comprise the following steps：
A, titanium nitride is collected：Air velocity is adjusted to more than 0.02m/s, the titanium nitride of generation is blown in collector, the time 5
~10min, collect titanium nitride；
B, continuous production：Air velocity is adjusted to 0.003~0.02m/s, titanium valve is added and continues to nitrogenize.
8. preparation method as claimed in claim 7, it is characterized in that：Step a by titanium nitride blow to time of collector for 5~
10min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711206023.8A CN107804830A (en) | 2017-11-27 | 2017-11-27 | The preparation method of titanium nitride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711206023.8A CN107804830A (en) | 2017-11-27 | 2017-11-27 | The preparation method of titanium nitride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107804830A true CN107804830A (en) | 2018-03-16 |
Family
ID=61581783
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711206023.8A Pending CN107804830A (en) | 2017-11-27 | 2017-11-27 | The preparation method of titanium nitride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107804830A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108677025A (en) * | 2018-07-12 | 2018-10-19 | 重庆大学 | The method that titanium-containing blast furnace slag carries titanium |
| CN112475309A (en) * | 2020-12-15 | 2021-03-12 | 江苏金物新材料有限公司 | Method for preparing spherical titanium nitride powder by reaction atomization method |
| RU2807847C1 (en) * | 2023-10-09 | 2023-11-21 | федеральное государственное автономное образовательное учреждение высшего образования "Пермский национальный исследовательский политехнический университет" | Method for producing stoichiometric titanium nitride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3416891A (en) * | 1964-11-27 | 1968-12-17 | Centre Nat Rech Scient | Solid solutions of the transition metal nitrides and oxinitrides and methods of preparation thereof |
| CN104498982A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium nitride |
-
2017
- 2017-11-27 CN CN201711206023.8A patent/CN107804830A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3416891A (en) * | 1964-11-27 | 1968-12-17 | Centre Nat Rech Scient | Solid solutions of the transition metal nitrides and oxinitrides and methods of preparation thereof |
| CN104498982A (en) * | 2015-01-07 | 2015-04-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing titanium nitride |
Non-Patent Citations (3)
| Title |
|---|
| 《中国建设科技文库》编委会编: "《中国建设科技文库 建筑材料卷（1998）》", 30 September 1998, 中国建材工业出版社 * |
| KYEONG-OOK LEE ET AL.: "FLUIDIZED-BED COMBUSTION SYNTHESIS OF TITANIUM NITRIDE", 《PROCEEDINGS OF THE COMBUSTION INSTITUTE》 * |
| 裴立宅 编著: "《高技术陶瓷材料》", 30 June 2015, 合肥工业大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108677025A (en) * | 2018-07-12 | 2018-10-19 | 重庆大学 | The method that titanium-containing blast furnace slag carries titanium |
| CN112475309A (en) * | 2020-12-15 | 2021-03-12 | 江苏金物新材料有限公司 | Method for preparing spherical titanium nitride powder by reaction atomization method |
| RU2807847C1 (en) * | 2023-10-09 | 2023-11-21 | федеральное государственное автономное образовательное учреждение высшего образования "Пермский национальный исследовательский политехнический университет" | Method for producing stoichiometric titanium nitride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101717117B (en) | Method for producing vanadium trioxide | |
| CN103130506B (en) | Method for preparing superfine titanium carbonitride | |
| CN106044771B (en) | A kind of titanium carbide preparation method that titanium processing is proposed based on titanium-containing blast furnace slag carbonization | |
| CN101392333B (en) | Vanadium-nitrogen alloy preparation method and device | |
| CN108358205B (en) | Ti3SiC2Powder synthesis method | |
| CN108557783A (en) | The preparation method of high-purity nm titanium nitride powder | |
| CN107804830A (en) | The preparation method of titanium nitride | |
| CN103073320A (en) | Preparation method for ZrB2-SiC (w) ceramic raw material | |
| NO20081468L (en) | Ore reduction process and titanium oxide and iron metallization product | |
| CN106517202A (en) | Preparation method of titanium carbide slag | |
| Yin et al. | Kinetic study on the direct nitridation of silicon powders diluted with α-Si 3 N 4 at normal pressure | |
| CN109399585A (en) | A method of preparing titanium carbonitride | |
| CN105905902B (en) | A kind of production method for the titanium material that is carbonized | |
| CN106744960B (en) | A method of oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction | |
| CN109437917B (en) | Method for producing titanium nitride and titanium carbonitride by two-stage reduction nitridation | |
| CN107285288A (en) | The preparation method of nano silicon nitride powders | |
| CN106987725A (en) | A kind of titanium-containing blast furnace slag ferrosilicon process titanium extracting technology method | |
| CN104495845B (en) | A kind of pure Fe3the preparation technology of C block | |
| CN205152329U (en) | Sectional type graphite carbonization vapour deposition stove for silicone coating | |
| CN104846258B (en) | The preparation method of iron-based (V, Ti) CN composite granule | |
| CN103361448A (en) | Method of preparing Fe-Ca-Si alloy from melt metallurgical slag | |
| CN101734659B (en) | Method for preparing titanium carbide powder by high-frequency induction-carbothermic reduction | |
| CN102864273A (en) | Method for increasing converter gas CO recycling amount | |
| CN108409327A (en) | A kind of method of carbothermic method synthesis WC base nano composite powders | |
| CN107904658A (en) | A kind of reduction furnace inner wall preparation method of composite coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180316 |
|
| RJ01 | Rejection of invention patent application after publication |