CN112125308B - Method for preparing titanium carbide - Google Patents
Method for preparing titanium carbide Download PDFInfo
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- CN112125308B CN112125308B CN202010981869.4A CN202010981869A CN112125308B CN 112125308 B CN112125308 B CN 112125308B CN 202010981869 A CN202010981869 A CN 202010981869A CN 112125308 B CN112125308 B CN 112125308B
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/921—Titanium carbide
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
- C01B17/745—Preparation from sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a preparation method of titanium carbide. The preparation method comprises the following steps: placing the graphite crucible containing the ferrotitanium binary alloy in a vacuum reaction furnace for heating so as to melt the ferrotitanium binary alloy and carry out a combination reaction to obtain a combination product; quenching the combined product to obtain a quenched product; and performing acid leaching treatment on the quenched product to remove metallic iron, thereby obtaining titanium carbide. The preparation method utilizes the in-situ synthesis method to prepare the titanium carbide, the granularity of the product is not influenced by the granularity of the raw materials, and the Fe and the sulfuric acid in the raw materials can be recycled, so the production cost is lower.
Description
Technical Field
The invention relates to the field of titanium carbide synthesis, and particularly relates to a preparation method of titanium carbide.
Background
Titanium carbide has a NaCl type cubic crystal system structure, the unit cell parameter is 0.4327nm, the space group is Fm3m, and the titanium carbide has the characteristics of high melting point, high hardness, wear resistance and corrosion resistance, and also has good thermal conductivity, electrical conductivity and chemical stability, so the titanium carbide is widely applied to composite ceramic materials, aerospace materials, cutting tools, wear-resistant materials and the like. At present, the method for preparing titanium carbide at home and abroad mainly comprises the carbothermic reduction of TiO2Methods, direct reaction methods, sol-gel methods, microwave synthesis methods, mechanical ball milling methods, chemical vapor deposition methods, and the like. Titanium dioxide and carbon black are generally used as raw materials in industry, and the titanium carbide is prepared by carbothermic reduction for 24 hours at 1700-2100 ℃. In the production process, the contact area of titanium dioxide and carbon black is small, the distribution is uneven, and the chemical combination reaction is not favorably carried out.
The prior document (CN103936007) provides a method for preparing a nano-scale titanium carbide powder material, which comprises the steps of uniformly mixing nano-scale titanium dioxide powder and asphalt or phenolic resin according to a weight ratio of 1: 1-1.5, and preserving heat for 3-5 hours at a temperature of 150-300 ℃ under the protection of argon; uniformly mixing the cooled product with magnesium powder according to the weight ratio of 1: 0.2-0.4, calcining for 4-7 hours at the temperature of 600-700 ℃ under the protection of argon, washing by dilute hydrochloric acid after cooling, filtering and drying to finally obtain the nano-scale titanium carbide powder. The disadvantages are: (1) the carbon source used in the method is asphalt or phenolic resin, and the carbon source needs to be mixed with titanium dioxide powder to prepare a precursor product. The precursor product is required to be mixed with magnesium powder for reduction reaction, and finally the titanium carbide is prepared through magnesiothermic reduction and carbothermic reduction. Asphalt, phenolic resin and magnesium powder are expensive, and the magnesium powder cannot be reused, so that the production cost is high. (2) The particle size of the product titanium carbide is influenced by the particle size of the raw material titanium dioxide, and the nano-scale titanium dioxide powder is required to be used for preparing the nano-scale titanium carbide powder.
Another prior document (CN105567970A) provides a process for preparing titanium carbide by using ilmenite, a smelting process and application thereof. The technology uses ilmenite and carbon powder as raw materials, the ilmenite and the carbon powder are uniformly mixed and then pressed into blocks, a chemical combination reaction is carried out in a vacuum furnace to obtain iron and titanium carbide powder, and the titanium carbide powder can be obtained after solution leaching; the purity of the obtained titanium carbide is more than 98 percent, and the granularity is less than 10 mu m; the vacuum carbothermic product iron and titanium carbide powder can be used for preparing Fe-TiC composite materials. The disadvantages are that: the raw materials have more impurities, the granularity of the titanium carbide particles prepared by the method is micron-sized, the particles are limited by the granularity of ilmenite, the nano-scale titanium carbide is difficult to prepare, and the reaction process belongs to solid-solid reaction.
In view of the above problems, it is desirable to provide a method for producing titanium carbide that is not affected by the particle size of the reaction raw material.
Disclosure of Invention
The invention mainly aims to provide a preparation method of titanium carbide, which aims to solve the problems that the granularity of the titanium carbide is limited by the granularity of raw materials and a nano-scale titanium carbide product is difficult to prepare in the existing preparation method of the titanium carbide.
In order to achieve the above object, the present invention provides a method for preparing titanium carbide, comprising: placing the graphite crucible containing the ferrotitanium binary alloy in a vacuum reaction furnace, heating to melt the ferrotitanium binary alloy and carrying out a combination reaction to obtain a combination product; quenching the combined product to obtain a quenched product; and carrying out acid leaching treatment on the quenched product to remove metallic iron and obtain titanium carbide.
Further, the temperature of the combination reaction is 1400-1700 ℃, the reaction time is 10-30 min, and the vacuum degree is lower than 0.1 Pa.
Further, the temperature of the combination reaction is 1500-1600 ℃, the reaction time is 10-30 min, and the vacuum degree is less than 0.01 Pa.
Further, the combination reaction process is a temperature programming process; preferably, the rate of the temperature programming process is 5-10 ℃/min.
Furthermore, the content of titanium element in the ferrotitanium binary alloy is 5-30%.
Further, the quenching treatment process comprises the following steps: quenching the reduction product by using inert gas to obtain a quenched product; preferably, the inert gas is selected from one or more of the group consisting of helium, neon, argon, krypton and xenon.
Further, the quenching treatment process comprises the following steps: and quenching the reduction product in a vacuum environment to obtain a quenched product.
Further, the acid leaching treatment comprises: leaching the quenched product by using sulfuric acid; preferably, the concentration of the sulfuric acid is 0.5-2 mol/L.
By applying the technical scheme of the invention, the ferrotitanium alloy and the high-purity graphite crucible are used as raw materials, and in the process of heating, the metallic iron and the carbon element in the graphite crucible form an Fe-C binary low-melting-point liquid phase. After the ferrotitanium alloy is completely melted, the carbon element can be uniformly dispersed in the metal liquid phase, and the titanium element and the carbon element can form a compound product containing nano-scale titanium carbide through an in-situ generation method. After the reaction is completed, the above-mentioned compound product is quenched to suppress further increase in the particle diameter of the titanium carbide particles. Because the quenched product also contains a certain amount of metallic iron, the iron in the quenched product needs to be removed through an acid leaching process to obtain the required titanium carbide product. The preparation method utilizes the in-situ synthesis method to prepare the titanium carbide, the granularity of the product is not influenced by the granularity of the raw materials, and the Fe and the sulfuric acid in the raw materials can be recycled, so the production cost is lower.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic structural view of an apparatus for producing titanium carbide according to a preferred embodiment of the present invention; and
fig. 2 shows a process flow diagram of a method for producing titanium carbide provided in example 1 of the present invention.
Wherein the figures include the following reference numerals:
10. a quenching zone; 11. a first housing; 12. an electromagnetic gate; 101. an inert gas inlet; 20. a vacuum heating zone; 21. a second housing; 30. a lifting device; 40. a graphite crucible; 50. a heating assembly; 60. an inert gas source; 70. a vacuum pump.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the particle size of titanium carbide in the existing titanium carbide preparation method is limited by the particle size of raw materials, and the problem of difficult preparation of nano-scale titanium carbide products is solved. In order to solve the above technical problem, the present application provides a method for preparing titanium carbide, including: placing a graphite crucible containing ferrotitanium binary alloy in a vacuum reaction furnace, heating to melt the ferrotitanium binary alloy and carrying out a combination reaction to obtain a combination product; quenching the combined product to obtain a quenched product; and carrying out acid leaching treatment on the quenched product to remove metallic iron and obtain titanium carbide.
The ferrotitanium alloy and the high-purity graphite crucible are used as raw materials, and in the process of temperature rise, the metallic iron and the carbon element in the graphite crucible form an Fe-C binary low-melting-point liquid phase. After the ferrotitanium alloy is completely melted, the carbon element can be uniformly dispersed in the metal liquid phase, and the titanium element and the carbon element can form a compound product containing nano-scale titanium carbide through an in-situ generation method. After the reaction is completed, the above-mentioned compound product is quenched to suppress further increase in the particle diameter of the titanium carbide particles. Because the quenched product also contains a certain amount of metallic iron, the iron in the quenched product needs to be removed through an acid leaching process to obtain the required titanium carbide product. The preparation method utilizes the in-situ synthesis method to prepare the titanium carbide, the granularity of the product is not influenced by the granularity of the raw materials, and the Fe and the sulfuric acid in the raw materials can be recycled, so the production cost is lower.
Preferably, in order to prevent the high-purity graphite crucible from being damaged, the graphite crucible with larger thickness or a protective crucible sleeved outside the graphite crucible can be used to prevent the high-temperature melt from leaking.
The temperature of the combination reaction process is higher than the melting point of the ferrotitanium binary alloy. In a preferred embodiment, the temperature of the combination reaction is 1400-1700 ℃, the reaction time is 10-30 min, and the vacuum degree is lower than 0.1 Pa. The temperature and reaction time of the reaction include, but are not limited to, the above ranges, and limiting it to the above ranges facilitates further refinement of the particle size of titanium carbide while increasing the yield of titanium carbide. More preferably, the temperature of the combination reaction is 1500-1600 ℃, the reaction time is 10-30 min, and the vacuum degree is less than 0.01 Pa.
In a preferred embodiment, the combination reaction process is a temperature programmed process. The reduction process can be carried out in a stable state by means of temperature programming, and the dispersion degree of carbon elements in the ferrotitanium alloy molten liquid is further improved, so that the contact area of the carbon elements and the ferrotitanium alloy molten liquid is improved, the granularity of the ferrotitanium alloy is further refined, and more preferably, the speed of the temperature programming process is 5-10 ℃/min.
In a preferred embodiment, the content of titanium element in the ferrotitanium binary alloy is 5-30%.
The quenching treatment process can adopt a method commonly used in the field as long as other impurity elements are not introduced, and the specific steps adopted by the quenching treatment process are not limited. In a preferred embodiment, the quenching process comprises: quenching the combined product by using inert gas to obtain a quenched product; preferably, the inert gas is selected from one or more of the group consisting of helium, neon, argon, krypton and xenon. In another preferred embodiment, the quenching process comprises: and quenching the reduction product in a vacuum environment to obtain a quenched product.
The quenched product also contains a certain amount of metallic iron, so that the iron in the quenched product needs to be removed by an acid leaching process to obtain a desired titanium carbide product. The acid leaching treatment comprises the following steps: dipping the quenching product by using sulfuric acid; preferably, the concentration of the sulfuric acid is 0.5-2 mol/L. Of course, the product of the above combination reaction process can also be directly used for preparing Fe-TiC composite material.
In order to further reduce the production cost, in a preferred embodiment, the preparation method further comprises: evaporating the leachate obtained in the acid leaching process to obtain a ferrous sulfate solution; and (3) placing the ferrous sulfate solution in a reaction furnace, and heating to 650 ℃ to obtain ferric trioxide and mixed gas of sulfur dioxide and sulfur trioxide. The mixed gas can be used for preparing sulfuric acid and reused in the leaching process. Fe2O3Can be further used for extracting iron.
The present application also provides a titanium carbide preparation apparatus, as shown in fig. 1, the titanium carbide preparation apparatus includes: a quenching zone 10, a vacuum heating zone 20, a lifting device 30 and a graphite crucible 40. The quenching zone 10 is located above the vacuum heating zone 20, the graphite crucible 40 is located inside the titanium carbide preparation device, and the height of the graphite crucible 40 is adjusted by the lifting device 30. Preferably, the vacuum heating zone 20 includes a second housing 21, a heating assembly 50 disposed inside the second housing 21; the quenching area 10 comprises a first shell 11, an electromagnetic door 12, the electromagnetic door 12 is used for separating the quenching area 10 from a vacuum heating area 20, and an inert gas inlet 101 and a lifting motor connecting port are arranged on the first shell 11. Preferably, the titanium carbide preparation apparatus further comprises an inert gas source 60 and a vacuum pump 70, wherein the vacuum pump 70 is communicated with the vacuum heating zone 20, and the inert gas source 60 is communicated with the inert gas inlet 101.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example titanium carbide was prepared using the apparatus shown in figure 1 and the process flow diagram is shown in figure 2.
Example 1
And (3) putting the FeTi alloy into a high-purity graphite crucible, wherein the mole fraction of Ti in the FeTi alloy is 5%. And (3) pumping the vacuum degree in the vacuum reaction furnace to 0.01Pa, closing an electromagnetic gate, raising the temperature of the reaction furnace to 1500 ℃ at a temperature rise rate of 10 ℃, and preserving the temperature for 20min to carry out a combination reaction to obtain a combination product.
And after the heat preservation is finished, closing the temperature rising program, opening the electromagnetic door, rising the graphite crucible to a quenching area, and spraying high-purity argon gas for quenching to obtain a quenching product.
And (3) carrying out acid leaching on the quenched product by using 1mol/L sulfuric acid to remove metallic iron, so as to obtain titanium carbide particles with the particle size of 130 nm. Evaporating the leaching solution to obtain FeSO4. FeSO (ferric oxide) is added4Placing the mixture into a reaction furnace and heating the mixture to 600 ℃ to obtain Fe2O3And SO2And SO3The mixed gas of (2). The mixed gas can be used for preparing sulfuric acid and reused in the leaching process. Fe2O3Can be further used for extracting iron.
Example 2
The FeTi alloy is put into a high-purity graphite crucible, and the mole fraction of Ti in the FeTi alloy is 20%. And (3) pumping the vacuum degree in the vacuum reaction furnace to 0.1Pa, closing an electromagnetic gate, raising the temperature of the reaction furnace to 1600 ℃ at a temperature rise rate of 10 ℃, and preserving the temperature for 30min to carry out a combination reaction to obtain a combination product.
After the heat preservation is finished, closing the temperature rising program, opening the electromagnetic door, rising the graphite crucible to a quenching area, spraying high-purity argon gas into the quenching area, and quenching to obtain a quenching product.
And (3) carrying out acid leaching on the quenched product by using 2mol/L sulfuric acid to remove metallic iron, so as to obtain titanium carbide particles with the particle size of 160 nm. Evaporating the leachate to obtainTo FeSO4. FeSO (ferric oxide) is added4Placing into a reaction furnace and heating to 650 ℃ to obtain Fe2O3And SO2And SO3The mixed gas of (1). The mixed gas can be used for preparing sulfuric acid and reused in the leaching process. Fe2O3Can be further used for extracting iron.
Example 3
The differences from example 2 are: the temperature of the reaction furnace is increased to 1400 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 10 min.
The obtained product is titanium carbide particles with the particle size of 200 nm.
Example 4
The differences from example 2 are: heating to 1600 ℃ at the temperature rising rate of 10 ℃, and preserving the heat for 120min to carry out the combination reaction.
The obtained product is 500nm titanium carbide particles.
Example 5
The differences from example 2 are: the temperature is raised to 1600 ℃ at the temperature rising rate of 10 ℃, and the temperature is kept for 5min to carry out the combination reaction.
The obtained product is 150nm titanium carbide particles. However, some Ti in the FeTi alloy is not reacted completely.
Example 6
The differences from example 2 are: the degree of vacuum in the chemical combination reaction was 1 MPa.
The resulting product was 150nm titanium carbide particles, but contained some TiCN particles, affecting the titanium carbide purity.
Example 7
The differences from example 2 are: in the ferrotitanium binary alloy, the content of titanium element is 40%.
The obtained product is titanium carbide particles with the particle size of 600 nm.
Example 8
The differences from example 2 are: in the ferrotitanium binary alloy, the content of titanium element is 1 percent.
The obtained product is 150nm titanium carbide particles, and the yield is too low, so that the expanded production is not facilitated.
Comparative example 1
And implementation ofThe differences in example 1 are: using FeTiO3Instead of the FeTi alloy.
The resulting product was 150 μm titanium carbide particles.
Comparative example 2
The differences from example 1 are: graphite crucibles are not used as carbon sources, but carbon powder is directly used as the carbon source.
The resulting product was 200 μm titanium carbide particles.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
comparing examples 1 to 8 and comparative examples 1 to 2, it can be seen that a nano-sized titanium carbide material can be prepared by the preparation method provided by the present application.
It is understood from comparative examples 2 to 6 that it is advantageous to refine the grain size of the titanium carbide material by limiting the target temperature, holding time, and degree of vacuum in the combination reaction to the preferable ranges in the present application.
It is understood from comparative examples 2 and 7 to 8 that limiting the content of titanium element in the ferrotitanium binary alloy to the preferred range in the present application is advantageous for refining the grain size of the titanium carbide material.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for producing titanium carbide, characterized by comprising:
placing a graphite crucible containing ferrotitanium binary alloy in a vacuum reaction furnace, heating to melt the ferrotitanium binary alloy and carrying out a combination reaction to obtain a combination product; the temperature of the combination reaction is 1400-1700 ℃, the reaction time is 10-30 min, and the vacuum degree is lower than 0.1 Pa;
quenching the combined product to obtain a quenched product; and
and carrying out acid leaching treatment on the quenched product to remove metallic iron, so as to obtain the titanium carbide.
2. The preparation method according to claim 1, wherein the temperature of the combination reaction is 1500-1600 ℃, the reaction time is 10-30 min, and the vacuum degree is less than 0.01 Pa.
3. The method of claim 1, wherein the combination reaction process is a temperature-programmed process.
4. The method according to claim 3, wherein the temperature programming process is performed at a rate of 5 to 10 ℃/min.
5. The method according to any one of claims 1 to 4, wherein the content of titanium in the ferrotitanium binary alloy is 5 to 30%.
6. The method of manufacturing according to claim 5, wherein the quenching process includes:
and quenching the combined product by adopting inert gas to obtain the quenched product.
7. The method of claim 6, wherein the inert gas is one or more selected from the group consisting of helium, neon, argon, krypton, and xenon.
8. The production method according to claim 5, wherein the quenching process includes: and quenching the combined product in a vacuum environment to obtain the quenched product.
9. The method according to claim 5, wherein the acid leaching treatment comprises: leaching the quenched product with sulfuric acid.
10. The method according to claim 9, wherein the concentration of the sulfuric acid is 0.5 to 2 mol/L.
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