CN109019625B - Method for preparing titanium boride powder - Google Patents
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- CN109019625B CN109019625B CN201811156089.5A CN201811156089A CN109019625B CN 109019625 B CN109019625 B CN 109019625B CN 201811156089 A CN201811156089 A CN 201811156089A CN 109019625 B CN109019625 B CN 109019625B
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- C01B35/00—Boron; Compounds thereof
- C01B35/02—Boron; Borides
- C01B35/04—Metal borides
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Abstract
The invention belongs to the field of titanium material preparation, and particularly relates to a preparation method of titanium boride powder. The invention aims to solve the technical problems that the preparation method of titanium boride powder in the prior art has complex steps, low production efficiency and high cost. The technical scheme of the invention provides a method for preparing titanium boride powder, which comprises the following steps: with TiCl4、BCl3Taking metal magnesium as a reducing agent and magnesium chloride as a reaction medium, and adding TiCl4、BCl3The gaseous mixture is introduced into molten salt formed by heating a mixture of metal magnesium and magnesium chloride, and TiB is prepared by one-step synthesis by a magnesiothermic reduction method2And (3) powder. The method has simple steps and low equipment requirement, does not need to use high-price raw materials such as titanium powder, boron powder and the like, and can obviously reduce the production cost. The product prepared by the method has high purity, less impurity residue, proper particle size and good application prospect.
Description
Technical Field
The invention belongs to the field of titanium material preparation, and particularly relates to a preparation method of titanium boride powder.
Background
Titanium boride (TiB)2) The material is a novel multifunctional material, has the advantages of high strength, high hardness, high temperature resistance, acid and alkali corrosion resistance, wear resistance, good electrical conductivity, thermal conductivity and the like, and is widely used for preparing metal ceramics, cutting tools, dies and crucibles for smelting metals as a reinforcing phase of a composite material. In addition, the titanium boride has the characteristics of high melting point, good conductivity, high temperature resistance and aluminum liquid and cryolite corrosion resistance, so that the titanium boride becomes an ideal material for an aluminum electrolysis cathode.
The prior preparation methods of titanium boride mainly comprise direct synthesis methods, carbothermic methods, metallothermic methods, vapor deposition methods and the like.The direct synthesis method has high preparation cost because titanium powder and boron powder are used as raw materials; when carbon, titanium dioxide and boron oxide are used as raw materials and prepared by adopting a carbothermic reduction method, the reaction temperature is higher, and the prepared TiB2Carbon impurity residue exists in the waste water; metallothermic process, i.e. high temperature self-propagating synthesis process (SHS), using magnesium, aluminium as reducing agent and TiO2Synthesizing TiB by taking boron oxide as a boron source and taking titanium oxide as a titanium source2The reaction is automatically carried out after initiation, heating is not needed, but Mg and Al are easy to remain in the synthesized product, and the powder granularity is larger; the vapor deposition method is TiCl4 and BCl3As raw material, with H2The reducing agent is obtained, the obtained product has high purity and fine grain diameter, but the production efficiency is low and the cost is higher.
Chinese patent document CN103265048A discloses a TiB2Preparation method of superfine powder material from Mg powder and B2O3Powder, TiO2NaCl as raw material and adopting high-temperature self-propagating method to prepare TiB2Powder, but the synthesized product is easy to remain Mg and Al, and the particle size of the powder is larger. CN 102584242A discloses a high-temperature high-pressure preparation method of titanium diboride, which takes Ti powder and boron powder as raw materials to prepare TiB by a metal hot-pressing sintering method2Because titanium powder and boron powder are used as raw materials, the preparation cost is higher. CN108439422A discloses a method for preparing titanium boride alloy by aluminothermic reduction, which takes sodium fluotitanate, sodium fluoborate and aluminum powder as raw materials and adopts aluminothermic reduction and vacuum distillation methods to prepare the titanium boride alloy.
Disclosure of Invention
The invention aims to solve the technical problems that the preparation method of titanium boride powder in the prior art has the defects of complex steps, low production efficiency and high cost. The technical scheme for solving the technical problems is to provide a method for preparing titanium boride powder. The method comprises the following steps:
with TiCl4、BCl3Taking metal magnesium as a reducing agent and magnesium chloride as a reaction medium, and adding TiCl4、BCl3Introducing the gaseous mixture into a mixture of metal magnesium and magnesium chlorideIn the magnesium chloride fused salt formed by combined heating, the TiB is prepared by one-step synthesis by a magnesiothermic reduction method2And (3) powder.
Further, the method comprises the following steps:
a. adding metal magnesium and magnesium chloride into a reaction container, adding the metal magnesium and the magnesium chloride in a molar ratio of 1-4: 1, and heating the reaction container to 750-800 ℃;
b. mixing TiCl4And BCl3Mixing to control TiCl4And BCl3In a molar ratio of 1: 2; mixing the TiCl4And BCl3Heating to 300-500 ℃, and slowly introducing MgCl into the lower part of the reaction vessel in a gaseous state2Carrying out reaction in molten salt; mg in the reaction vessel and the introduced TiCl4、BCl3The ratio of the component (A) to the component (B) is controlled to be 5-12: 1: 2;
c. cooling, cleaning and drying the reaction product to obtain TiB2And (3) powder.
Preferably, the ratio of Mg to MgCl2 in step a is 1: 1. In the step b, Mg and the introduced TiCl in the reaction container4、BCl3The molar ratio of (a) to (b) is preferably 10 to 12:1: 2.
In the reaction process, the materials in the reaction container are stirred at the stirring speed of 10-20 rpm (revolutions per minute).
Wherein, the reaction vessel in the method is a closed reaction vessel with pressure relief function.
Wherein, in the method, inert gas is used for protecting the atmosphere of the reaction system in the reaction process. Argon is preferred in view of economy.
Wherein, in the method, when the pressure exceeds 20KPa in the reaction process, the pressure of the reaction vessel is relieved.
The cleaning step of the reaction product in the method is to soak the reaction product in 8-12 mol/L hydrochloric acid and then to wash the reaction product with distilled water.
The drying in the method is drying at 100-120 ℃.
The invention has the beneficial effects that:
the inventionThe method takes magnesium metal as a reducing agent and TiCl4And BCl3The mixture is taken as raw material and MgCl is taken2One-step preparation of TiB by Mg thermal reduction using molten salt as reaction medium2And (3) powder. The method has simple steps and low equipment requirement, does not need to use high-price raw materials such as titanium powder, boron powder and the like, and can obviously reduce the production cost. The product prepared by the method has high purity, less impurity residue and purity higher than 99.5 percent; directly obtained TiB2The granularity of the powder is more than 65 percent when the particle size is 300-1000 nm, and TiB can be controlled2The powder has good application prospect due to the size of the powder.
Detailed Description
The method takes metal magnesium as a reducing agent and TiCl4And BCl3The mixture is taken as raw material, MgCl is added2Direct preparation of TiB of suitable particle size by thermal reduction of Mg as reaction medium2And (3) powder. In the process of the present invention, TiCl is reacted4And BCl3The mixture is first reacted with MgCl as reaction medium2Contact with MgCl2Complexed and dissolved in MgCl2The metal Mg in the alloy is further mixed with TiCl4、BCl3Respectively carrying out reduction reaction, and combining the reduced metal Ti with B to obtain TiB2And deposited in the container as a powder. Due to the reduction of TiCl4And BCl3The reaction rate and the heat release when the mixed salt reacts with Mg effectively avoid the reduction product TiB2Sintering takes place, so that TiB can be obtained directly in one step2And (3) powder. When using TiCl of higher purity4、BCl3When the raw materials are equal, high-purity TiB can be conveniently prepared2And (3) powder.
The main reaction equation of the method is as follows: 5Mg + TiCl4+2BCl3＝TiB2+5MgCl2。
The method comprises the following steps:
with TiCl4、BCl3Taking metal magnesium as a reducing agent and magnesium chloride as a reaction medium, and adding TiCl4、BCl3The gaseous mixture is introduced into a molten salt formed by heating a mixture of metal magnesium and magnesium chloride, andone-step synthesis of TiB by magnesiothermic reduction method2And (3) powder.
Specifically, the method comprises the following steps:
a. adding metal magnesium and magnesium chloride into a reaction container, adding the metal magnesium and the magnesium chloride in a molar ratio of 1-4: 1, and heating the reaction container to 750-800 ℃;
b. mixing TiCl4And BCl3Mixing to control TiCl4And BCl3In a molar ratio of 1: 2; mixing the TiCl4And BCl3Heating to 300-500 ℃, and slowly introducing MgCl into the lower part of the reaction vessel in a gaseous state2Carrying out reaction in molten salt; mg in the reaction vessel and the introduced TiCl4、BCl3The ratio of the component (A) to the component (B) is controlled to be 5-12: 1: 2;
c. cooling, cleaning and drying the reaction product to obtain TiB2And (3) powder.
Preferably, the ratio of Mg to MgCl2 in step a is 1: 1. In the step b, Mg and the introduced TiCl in the reaction container4、BCl3The molar ratio of (a) to (b) is preferably 10 to 12:1: 2.
A key point of the process of the invention is that TiCl is reacted4And BCl3In gaseous form to Mg, MgCl2Molten salt MgCl at the bottom of the reaction vessel2Internally reacting TiCl4Mixing with BCl3 first with MgCl2Contact, then dissolve in MgCl2Metal Mg and TiCl in4、BCl3The reduction reaction is carried out after the contact, and then the metal Ti is synthesized into TiB by the B reaction2And deposited as a powder on the bottom of the container. Here MgCl2The reaction rate is reduced, and the reaction is also used as a cooling medium, so that TiB2 powder can be obtained; if TiCl is present4、BCl3The mixture reacts directly with Mg to obtain only blocky TiB2。
The form of the raw material magnesium and MgCl2 is not limited, and it is sufficient to put the raw material magnesium and MgCl2 directly into the reactor and raise the temperature without mixing them in advance.
Naturally, the gaseous TiCl is suitably controlled4And BCl3Rate of introduction of molten salt. Qi (Qi)In the form of TiCl4And BCl3When the introduction is fast, the reaction proceeds fast, the heat released by the reaction increases, and MgCl is present in the reactor2The molten salt temperature will increase and the product TiB2The sintering degree of the powder is increased, so that the particle size of the prepared powder is increased; slow introduction of the catalyst to smooth the reaction and generate TiB2The average particle size of the powder will be smaller. Thus, it is possible to control the TiCl gas4And BCl3The introduction rate is used to control the produced TiB to a certain extent2Particle size of the powder. Of course, in general, a small particle size of TiB is desired2Powder, thus it is necessary to mix gaseous TiCl4And BCl3The molten salt is introduced slowly as possible.
In the reaction process, the materials in the reaction container are stirred at the stirring speed of 10-20 rpm (revolutions per minute).
Wherein, the reaction vessel in the method is a closed carbon steel tank with pressure relief function. The closed carbon steel tank with pressure relief function is used to make the reaction able to withstand the temperature required by the reaction and to discharge excess gas in the system to maintain the pressure in the vessel at a suitable level when needed again. Other reaction vessels meeting the requirements can be used, for example, a stainless steel tank reaction vessel with pressure relief function and closed material 1Cr18Ni9Ti can also be used.
In order to ensure that the reaction can be smoothly carried out, the reaction system is protected by using argon in the reaction process.
Since the magnesium thermal reaction is an exothermic reaction and generates gas, the above method generally performs a pressure relief treatment of the reaction vessel when the pressure in the vessel exceeds 20KPa during the reaction.
Reduction of the resulting TiB2The powder was entrained with MgCl2 in order to remove TiB from the reaction product2The powder was separated from the system and the product was washed. The preferable cleaning mode is that after the cleaning agent is soaked in 8-12 mol/L hydrochloric acid, the cleaning agent is washed by water. In order to clean thoroughly and reduce impurity residue, the hydrochloric acid soaking is sufficient, and the rinsing water can be sufficiently rinsed by using distilled water.
Wherein, the drying is drying at 100-120 ℃. Drying the cleaned product to obtain TiB2 powder.
To ensure the purity of the product, TiCl4、BCl3The purity requirement of each is greater than 99.98%. The purity of Mg and MgCl is also better to be more than 99.99%.
The process of the present invention is described in more detail below by way of examples.
Example one preparation of TiB Using the method of the invention2Powder of
TiCl with purity of more than 99.98 percent4、BCl31.62Kg and 2.00Kg of each were mixed and heated to 500 ℃ for use.
Mg and MgCl with purity of more than 99.99 percent22.25Kg and 8.94Kg of each, and heating to 800 ℃; the MgCl2, Mg mixture was argon blanketed and stirred at 20 rpm.
Introducing gaseous TiCl4、BCl3The mixture is added into a closed carbon steel tank reaction vessel with the volume of 10L and the pressure relief function at the speed of 0.1Kg/min for reaction, and MgCl is introduced into the bottom of the vessel2In molten salt. In the reduction reaction process, forcibly cooling the reaction container in a blowing mode, and controlling the temperature of a reactor system at 780-800 ℃; when the pressure of the reactor is more than 20KPa, releasing the pressure of the reactor; until the reaction is fully completed, obtaining a reduction product at the bottom of the closed carbon steel tank reaction vessel, wherein the reaction time is about 45 minutes.
After the system is naturally cooled, the reduction product is soaked by hydrochloric acid with the concentration of 8mol/L for 2 hours, then washed by distilled water and dried at 120 ℃ to obtain TiB2And (3) powder. Through detection, the obtained TiB2The purity of the powder is more than 99.5%, and the granularity of the powder is more than 40% when the particle size is 300-1000 nm.
Example two preparation of TiB Using the method of the invention2Powder of
TiCl with purity of more than 99.98 percent4、BCl31.62Kg and 2.00Kg of each were mixed and heated to 500 ℃ for use.
Mg and MgCl with purity of more than 99.99 percent22.25Kg and 8 each.Mixing 94Kg and heating to 800 ℃; the MgCl2, Mg mixture was argon blanketed and stirred at 30 rpm.
Introducing gaseous TiCl4、BCl3Adding into a 10L reactor at a speed of 0.05Kg/min, and introducing MgCl into the bottom of the reactor2In molten salt. In the reduction reaction process, forced cooling is carried out on the reaction container by air blast, and the temperature of the reaction system is controlled to be 750-780 ℃. When the pressure of the reactor is more than 20KPa, releasing the pressure of the reactor; until the reaction is fully completed, obtaining a reduction product at the bottom of the closed carbon steel tank reaction vessel, wherein the reaction time is about 90 minutes.
Soaking the reduction product for 2 hours by using hydrochloric acid with the concentration of 8mol/L, then fully washing by using distilled water, and drying at 120 ℃ to obtain TiB2And (3) powder. Through detection, the obtained TiB2The purity of the powder is more than 99.5%, and the granularity of the powder is more than 68% when the particle size is 300-1000 nm.
Claims (7)
1. A preparation method of titanium boride powder is characterized by comprising the following steps: with TiCl4、BCl3Taking metal magnesium as a reducing agent and magnesium chloride as a reaction medium, and adding TiCl4、BCl3The gaseous mixture is introduced into magnesium chloride molten salt formed by mixing and heating metal magnesium and magnesium chloride, and TiB is prepared by one-step synthesis by a magnesiothermic reduction method2Powder; the method specifically comprises the following steps:
a. adding metal magnesium and magnesium chloride into a reaction container, adding the metal magnesium and the magnesium chloride in a molar ratio of 1-4: 1, and heating the reaction container to 750-800 ℃;
b. mixing TiCl4And BCl3Mixing to control TiCl4And BCl3In a molar ratio of 1: 2; mixing the TiCl4And BCl3Heating to 300-500 deg.C, introducing MgCl into the reactor at a rate of 0.05Kg/min or 0.1Kg/min in a gaseous state2Carrying out reaction in molten salt; mg in the reaction vessel and the introduced TiCl4、BCl3The ratio of (A) to (B) is controlled to be 5-12: 1: 2;
c. cooling, cleaning and baking the reaction productDrying to obtain TiB2And (3) powder.
2. The method for producing titanium boride powder according to claim 1, characterized in that: in the reaction process, materials in the reaction container are stirred at the stirring speed of 10-20 rpm.
3. The method for producing titanium boride powder according to claim 1, characterized in that: the reaction vessel is a closed reaction vessel with a pressure relief function.
4. The method for producing titanium boride powder according to claim 1, characterized in that: and inert gas is used for protecting the atmosphere of the reaction system in the reaction process.
5. The method for producing titanium boride powder according to claim 1, characterized in that: when the pressure exceeds 20KPa, the reaction vessel is subjected to pressure relief treatment.
6. The method for producing titanium boride powder according to claim 1, characterized in that: and the reaction product is cleaned by soaking in 8-12 mol/L hydrochloric acid and then washing with water.
7. The method for producing titanium boride powder according to claim 1, characterized in that: the drying is carried out at 100-120 ℃.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4503021A (en) * | 1983-04-26 | 1985-03-05 | The United States Of America As Represented By The Department Of Energy | Preparation of titanium diboride powder |
| CN101277775A (en) * | 2005-10-06 | 2008-10-01 | 国际钛金属粉末公司 | Titanium boride |
| JP4711724B2 (en) * | 2005-04-19 | 2011-06-29 | 学校法人同志社 | Electrolytic bath for molten salt plating and molten salt plating method using the electrolytic bath |
| CN105502398A (en) * | 2016-03-01 | 2016-04-20 | 郑州大学 | Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction |
| CN106834748A (en) * | 2017-04-19 | 2017-06-13 | 攀钢集团研究院有限公司 | A kind of method of continuous production titanium sponge |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4503021A (en) * | 1983-04-26 | 1985-03-05 | The United States Of America As Represented By The Department Of Energy | Preparation of titanium diboride powder |
| JP4711724B2 (en) * | 2005-04-19 | 2011-06-29 | 学校法人同志社 | Electrolytic bath for molten salt plating and molten salt plating method using the electrolytic bath |
| CN101277775A (en) * | 2005-10-06 | 2008-10-01 | 国际钛金属粉末公司 | Titanium boride |
| CN105502398A (en) * | 2016-03-01 | 2016-04-20 | 郑州大学 | Method for synthesizing tantalum carbide superfine powder through molten salt assisted magnesiothermic reduction |
| CN106834748A (en) * | 2017-04-19 | 2017-06-13 | 攀钢集团研究院有限公司 | A kind of method of continuous production titanium sponge |
Non-Patent Citations (2)
| Title |
|---|
| Gas-phase combustion synthesis of titanium boride (TiB2) nanocrystallites;R. L. Axelbaum et al.;《Journal of Materials Research》;19960430;第11卷(第4期);948-954 * |
| Low-temperature preparation of titanium diboride fine powder via magnesiothermic reduction in molten salt;Ke Bao et al.;《Journal of the American Ceramic Society》;20171231;第100卷;2266-2272 * |
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