CN113104822A - Method for reducing and nitriding titanium oxide - Google Patents
Method for reducing and nitriding titanium oxide Download PDFInfo
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- CN113104822A CN113104822A CN202110346584.8A CN202110346584A CN113104822A CN 113104822 A CN113104822 A CN 113104822A CN 202110346584 A CN202110346584 A CN 202110346584A CN 113104822 A CN113104822 A CN 113104822A
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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
- C01B21/076—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
- C01B21/0765—Preparation by carboreductive nitridation
Abstract
The invention relates to a method for reducing and nitriding titanium oxide, belonging to the technical field of metallurgy. The method for reducing and nitriding titanium oxide comprises the following steps: A. mixing titanium oxide: mixing carbon according to the mass ratio of 1: 2-2.5, and then carrying out ball milling; B. drying the ball-milled raw materials at a low temperature of 75-85 ℃ for 2.5-3.5 hours, and sieving the dried raw materials by using a sieve with 65-85 meshes; C.B, after sieving, taking oversize products to be fully mixed with hexamethylenetetramine, adding a polyvinyl alcohol solution to be mixed, and tabletting; D. and (3) placing the pressed article in a vacuum atmosphere, adjusting the pressure to 0.08-0.12 MPa by using nitrogen, and performing nitridation reaction at 1300-1400 ℃ for 2-3 hours. The process flow maximizes the contact surface of the raw materials, thereby maximizing the effect of the raw materials. The invention has the advantages of simple tabletting process flow, simple operation, low cost and high efficiency.
Description
Technical Field
The invention relates to a method for reducing and nitriding titanium oxide, belonging to the technical field of metallurgy.
Background
The production method of titanium nitride in industry has three general methods, mainly including titanium oxide reduction nitridation synthesis method, titanium powder nitridation method and gas phase method. However, in industry, low cost, high efficiency and low pollution are generally sought after. Therefore, a better method needs to be improved from the three methods. The titanium oxide reduction nitridation synthesis method has the characteristics of low cost, simple operation and facilities, large-scale production and wide raw material range. However, this method also has the disadvantages of high production temperature, small contact area of raw materials, and low activity.
Therefore, the improvement of the titanium oxide reduction nitridation synthesis method and the improvement of the activity of the titanium oxide reduction nitridation synthesis method have very important significance.
Disclosure of Invention
The invention aims to provide a novel method for reducing and nitriding titanium oxide.
In order to solve the technical problem of the invention, the method for reducing and nitriding titanium oxide comprises the following steps:
A. mixing titanium oxide: mixing carbon according to the mass ratio of 1: 2-2.5, and then carrying out ball milling;
B. drying the ball-milled raw materials at a low temperature of 75-85 ℃ for 2.5-3.5 hours, and sieving the dried raw materials with a 65-85-mesh sieve;
and C, sieving in the step B, fully mixing oversize products with hexamethylenetetramine, adding a polyvinyl alcohol solution, mixing and tabletting.
D. And (3) placing the pressed article in a vacuum atmosphere, adjusting the pressure to 0.08-0.12 MPa by using nitrogen, and performing nitridation reaction at 1300-1400 ℃ for 2-3 hours.
In a specific embodiment, the ball milling in the step A is performed for 3-4 hours at a speed of 450-480 r/min; the ball milling adopts a DECO-PBM-v-o-0.4L type vertical planetary ball mill.
In a specific embodiment, the mass ratio of the addition amount of hexamethylenetetramine to C is 1: 2-5.
In one embodiment, the polyvinyl alcohol solution is prepared by the following method: the dried polyvinyl alcohol powder was dissolved in deionized water.
The drying is to accurately weigh the amount of the polyvinyl alcohol powder, prevent water in the medicine from interfering the quality, and prevent the concentration of the prepared solution from not reaching the accurate concentration.
In a specific embodiment, the method for dissolving the polyvinyl alcohol powder in the deionized water is to heat the polyvinyl alcohol powder to 80-90 ℃ and stir the polyvinyl alcohol powder until the polyvinyl alcohol is completely dissolved.
In a specific embodiment, the mass of the polyvinyl alcohol powder is 0.3-0.8% of that of the deionized water.
In one embodiment, the sufficient mixing in step C is shaking and shaking for 5-25 minutes.
In a specific embodiment, the mass ratio of the addition amount of the polyvinyl alcohol solution in the step C to the titanium nitride is 1-10: 50-700.
In a specific embodiment, the compression pressure in the step C is 8-20 MP, and the compression time is 5-10 minutes.
In a specific embodiment, the material formed by the tabletting is a cylinder with the height of 10mm and the diameter of 20-30 mm.
Has the advantages that:
the process flow maximizes the contact surface of the raw materials, thereby maximizing the effect of the raw materials.
The invention has the advantages of simple tabletting process flow, simple operation, low cost, low efficiency and high efficiency
The method of the invention can produce titanium nitride on a large scale, so that the cost for producing the titanium nitride is lowered, and the quality and the yield of the produced titanium nitride are improved. The utilization of vanadium-titanium resources in China is maximized.
Drawings
FIG. 1 is a process diagram of a raw material manufacturing process of the present invention.
Detailed Description
In order to solve the technical problem of the invention, the method for reducing and nitriding titanium oxide comprises the following steps:
A. mixing titanium oxide: mixing carbon according to the mass ratio of 1: 2-2.5, and then carrying out ball milling;
B. drying the ball-milled raw materials at a low temperature of 75-85 ℃ for 2.5-3.5 hours, and sieving the dried raw materials with a 65-85-mesh sieve;
C.B, after sieving, taking oversize products to be fully mixed with hexamethylenetetramine, adding a polyvinyl alcohol solution to be mixed, and tabletting;
D. and (3) placing the pressed article in a vacuum atmosphere, adjusting the pressure to 0.08-0.12 MPa by using nitrogen, and performing nitridation reaction at 1300-1400 ℃ for 2-3 hours.
In a specific embodiment, the ball milling in the step A is performed for 3-4 hours at a speed of 450-480 r/min; the ball milling adopts a DECO-PBM-v-o-0.4L type vertical planetary ball mill.
In a specific embodiment, the mass ratio of the addition amount of hexamethylenetetramine to C is 1: 2-5.
In one embodiment, the polyvinyl alcohol solution is prepared by the following method: the dried polyvinyl alcohol powder was dissolved in deionized water.
The drying is to accurately weigh the amount of the polyvinyl alcohol powder, prevent water in the medicine from interfering the quality, and prevent the concentration of the prepared solution from not reaching the accurate concentration.
In a specific embodiment, the method for dissolving the polyvinyl alcohol powder in the deionized water is to heat the polyvinyl alcohol powder to 80-90 ℃ and stir the polyvinyl alcohol powder until the polyvinyl alcohol is completely dissolved.
In a specific embodiment, the mass of the polyvinyl alcohol powder is 0.3-0.8% of that of the deionized water.
In one embodiment, the sufficient mixing in step C is shaking and shaking for 5-25 minutes.
In a specific embodiment, the mass ratio of the addition amount of the polyvinyl alcohol solution in the step C to the titanium nitride is 1-10: 50-700.
In a specific embodiment, the compression pressure in the step C is 8-20 MP, and the compression time is 5-10 minutes.
In a specific embodiment, the material formed by the tabletting is a cylinder with the height of 10mm and the diameter of 20-30 mm.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Weighing dried polyvinyl alcohol (PVA) powder according to a proportion of 0.8% designed according to test requirements, slowly adding the powder into a beaker filled with deionized water to prepare a PVA solution, and then mixing 100g of titanium dioxide: mixing 220g of carbon, and putting the mixture into a vertical planetary ball mill for wet mixing at the rotating speed of 450r/min for 4 hours. After the ball milling is finished, the raw materials are put into a drying box with the temperature of 75 ℃ and dried for 3 hours at low temperature. And then, the dried raw materials are filtered by a 75-mesh sieve, and the constant-speed vibration and shaking are kept during the filtering, so that the raw materials are conveniently and uniformly mixed. After sieving, 20g of hexamethylenetetramine was added and mixed. And finally, after uniformly mixing, adding 7 drops of 0.8% PVA solution, shaking and mixing for 5 minutes, weighing and tabletting, wherein the tabletting time is 5 minutes, and the tabletting pressure is 20 MPa. Finally, a cylinder of 10mmX20 was obtained. Then the mixture is put into a hearth chamber with vacuum atmosphere, the pressure is adjusted to 0.12MP by nitrogen, and the temperature is adjusted to 1400 ℃ for nitridation reaction for 2.5 hours.
The process for preparing the raw materials is a short one-pass preparation, and has simple operation flow and low cost. The resulting final product was a 10mmX20 cylinder. The experiment finally obtains 71.350g of titanium nitride finished product in total, the obtained yield is 92.06%, more than 90% of the obtained products are titanium nitride, so the experiment greatly improves the yield of titanium nitride nitridation reaction.
Hexamethylenetetramine is white, is a hygroscopic crystalline powder, has an irritating odor and is flammable, has a melting point of 263 ℃, sublimes and decomposes at a temperature above the melting point, but does not melt. The smoke gas such as nitrogen oxide generated by sublimation is beneficial to the introduction of N element, and provides favorable conditions for the synthesis of TiN.
Claims (10)
1. A method for reductively nitriding titanium oxide, the method comprising:
A. mixing titanium oxide: mixing carbon according to the mass ratio of 1: 2-2.5, and then carrying out ball milling;
B. drying the ball-milled raw materials at a low temperature of 75-85 ℃ for 2.5-3.5 hours, and sieving the dried raw materials by using a sieve with 65-85 meshes;
C.B, after sieving, taking oversize products to be fully mixed with hexamethylenetetramine, adding a polyvinyl alcohol solution to be mixed, and tabletting;
D. and (3) placing the pressed article in a vacuum atmosphere, adjusting the pressure to 0.08-0.12 MPa by using nitrogen, and performing nitridation reaction at 1300-1400 ℃ for 2-3 hours.
2. The method for reductive nitridation of titanium oxide according to claim 1, wherein the ball milling in step a is performed at 450 to 480r/min for 3 to 4 hours; the ball milling is preferably carried out by a DECO-PBM-v-o-0.4L type vertical planetary ball mill.
3. The method for reductively nitriding titanium oxide according to claim 1 or 2, wherein the mass ratio of the amount of hexamethylenetetramine to C is 1:2 to 5.
4. The method for reductively nitriding titanium oxide according to any one of claims 1 to 3, wherein said polyvinyl alcohol solution is prepared by: the dried polyvinyl alcohol powder was dissolved in deionized water.
5. The method for reductive nitridation of titanium oxide according to claim 4, wherein the polyvinyl alcohol powder is dissolved in deionized water by heating to 80-90 ℃ and stirring until the polyvinyl alcohol is completely dissolved.
6. The method of titanium oxide reductive nitridation of claim 5, wherein the mass of polyvinyl alcohol powder is 0.3-0.8% of deionized water.
7. The method for reductively nitriding titanium oxide according to any one of claims 1 to 6, wherein the mixing in the step C is shaking and shaking for 5 to 25 minutes.
8. The method for reductive nitridation of titanium oxide according to any one of claims 1 to 6, wherein the mass ratio of the addition amount of the polyvinyl alcohol solution to the titanium nitride in step C is 1 to 10: 50-700.
9. The method for reductively nitriding titanium oxide according to any one of claims 1 to 7, wherein the pressure of the tablet in the step C is 8 to 20MP, and the tablet-pressing time is 5 to 10 minutes.
10. The method of claim 9, wherein the material formed by the tablet is a cylinder with a height of 10mm and a diameter of 20-30 mm.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951803A (en) * | 2005-10-17 | 2007-04-25 | 四川大学 | High temperature nitriding method for preparing nano crystalline titanium nitride ceramic superfine powder |
| US20160346773A1 (en) * | 2015-05-29 | 2016-12-01 | Uop Llc | Catalyst containing hydroxy metal oxide binder and process for preparing |
| CN108793101A (en) * | 2018-06-15 | 2018-11-13 | 昆明理工大学 | A kind of method that alumina carbon tropical resources reduction prepares aluminium nitride under vacuum |
| CN108927170A (en) * | 2018-08-17 | 2018-12-04 | 太原理工大学 | A kind of preparation method and application of the low-temperature denitration of flue gas catalyst based on CoMnAl houghite |
| JPWO2018061644A1 (en) * | 2016-09-30 | 2019-09-05 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion composition, curable composition, cured film, and production method thereof, color filter, solid-state imaging device, solid-state imaging device, infrared sensor |
-
2021
- 2021-03-31 CN CN202110346584.8A patent/CN113104822A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951803A (en) * | 2005-10-17 | 2007-04-25 | 四川大学 | High temperature nitriding method for preparing nano crystalline titanium nitride ceramic superfine powder |
| US20160346773A1 (en) * | 2015-05-29 | 2016-12-01 | Uop Llc | Catalyst containing hydroxy metal oxide binder and process for preparing |
| JPWO2018061644A1 (en) * | 2016-09-30 | 2019-09-05 | 富士フイルム株式会社 | Metal nitride-containing particles, dispersion composition, curable composition, cured film, and production method thereof, color filter, solid-state imaging device, solid-state imaging device, infrared sensor |
| CN108793101A (en) * | 2018-06-15 | 2018-11-13 | 昆明理工大学 | A kind of method that alumina carbon tropical resources reduction prepares aluminium nitride under vacuum |
| CN108927170A (en) * | 2018-08-17 | 2018-12-04 | 太原理工大学 | A kind of preparation method and application of the low-temperature denitration of flue gas catalyst based on CoMnAl houghite |
Non-Patent Citations (1)
| Title |
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| 橡胶工业原材料与装备简明手册编审委员会, 北京理工大学出版社 * |
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