CN106744960A - A kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction - Google Patents
A kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction Download PDFInfo
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Abstract
The invention provides a kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction,The method is using pure titinium dioxide or rutile as initial feed,From hydrogen and carbon dust respectively as reducing agent and carburization agent,Another effect of carbon dust is to reduce partial pressure of oxygen,Preparation temperature need to only reach relatively low 1200 ~ 1350 DEG C,During oxidation of coal titanium or/and titanium carbide is prepared there is gas-solid reduction reaction in hydrogen and titaniferous materials,Reduction efficiency is high,Reduction rate is fast,There is water gas reaction in the vapor produced after the carbon dust and hydrogen reducing that are fully mixed with raw material,Reduce the partial pressure of oxygen in material bed,So as to promote the carrying out of titanium oxide reduction reaction,Well mixed carbon dust also greatly improves carbonization efficiency simultaneously,Carbonation rate is fast,Realize the purpose of reduction and carbonization titanium oxide at a lower temperature,Save energy consumption cost,Preparation temperature is high in solving existing oxidation of coal titanium and titanium carbide production technology well,Low production efficiency,With high costs the problems such as.
Description
Technical field
The present invention relates to chemical metallurgy technical field, especially design it is a kind of with carburetted hydrogen gas reduction prepare oxidation of coal titanium or/and
The method of titanium carbide.
Background technology
Titanium carbide is a kind of with fusing point is high, the good characteristic such as hardness is high, chemical stability is good material, in industrial production
During be usually used to manufacture cermet, heat-resisting alloy and hard alloy, these products are in Aero-Space, coating material etc.
High-tech area has a very wide range of applications（Refer to document " Liu Yang, Zeng Lingke；Chinese pottery, 2002,38；7~10
Page "）.
The method of synthesizing titanium carbide has many kinds both at home and abroad at present, and industrial main utilization is carbothermic method.Document
“R. Koc, J.S. Folmer. Journal of Materials Science, 1997, 32:3101-3111 " and text
Offer " K Thorne, S J Ting. Journal of Materials Science, 1992,27:4406-4414 " is reported
TiO is reduced using carbon black2Powder obtains titanium carbide powder.But the problem that this method is present is also apparent from：Because reactant
Exist with scattered particle, the degree that reaction is carried out is subject to reactant contact area and carbon black in TiO2In distribution limitation,
Make to contain unreacted charcoal and TiO in product2, during reduction reaction, due to grain growth and interparticle chemical bonding,
The TiC powder of synthesis has particle size distribution wider, it is necessary to ball milling is processed；Reaction time is more long, about at 10 ~ 20 hours, instead
Due to being influenceed to make the powder of synthesis usually not pure enough by diffusion gradient in answering；React the temperature for needing also very high, about
1700 ~ 2100 DEG C, comprehensive energy consumption is very big.
Document " Feng Chengjian, Zhang Jianshu；Mineral products are comprehensively utilized, and 1997,6；34-41 pages " report contained using high-purity carbon reducing agent
Titanium blast furnace slag（TiO2：22%~23%）Produce titanium carbide.This method there is also some problems：React the temperature for needing higher, about
It is 1600 DEG C；Because TiC is a kind of high-temperature product, in carbonation reaction, the TiC of generation is outstanding in more scattered solia particle
Float in slag liquid, raise viscosity, prevent the reunion of TiC particulates, so the TiC granularities obtained after high temperature cabonization are too thin, and
And TiC particulates easily form abundance zone around carbon granules or iron shot, general milling method cannot make mineral reach effective monomer solution
From so as to cause later purification TiC more difficult.
Past many decades, in order to reduce the cost of titanium smelting process, the electrolysis with fused salt as medium extracts titanium technique
It is developed rapidly, and rapidly becomes the developing direction of titanium novel technology for extracting.Document " S.Q. Jiao, H.M. Zhu.
Journal of Alloys and Compounds, 2007, 438:243-246 " reports a kind of new carbon thermal reduction-molten
Salt electroextraction titanium technique（USTB techniques）, it is proposed that novel soluble electrolytic anode material oxidation of coal titanium（TiC x O y ,x+y=
1）.Facts have proved that this technique is a kind of very promising method in numerous Titanium new preparation processes.But preferable electrolytic anode
Preparation be the technique further development restrictive condition.In existing process flow, TiC is prepared x O y Method be carbon heat also
Former method, i.e., be reduced directly the TiO of high-purity using carbon dust2Powder, the course of reaction needs to carry out strict control to reaction condition
System, is otherwise difficult to generate TiC x O y , and the temperature of reaction requirement is very high, and reaction speed is slow, so energy consumption is also very
It is high.
In sum, the preparation method of current oxidation of coal titanium or/and titanium carbide, is on the one hand to utilize high pure raw material, this kind of
Method can obtain high-purity product, save follow-up purification process, but cost of material is high, and process energy consumption is greatly so as to make
Greatly improved into production cost；On the one hand it is to utilize TiO2The relatively low titaniferous materials of grade, although the temperature that this kind of method needs
It is relatively low, but follow-up purification process is sufficiently complex, and technological process is long, and production efficiency is relatively low.Therefore, need badly a kind of new
Low cost, low energy consumption, efficient oxidation of coal titanium or/and titanium carbide preparation technology.
The content of the invention
For above shortcomings in the prior art, reduced with carburetted hydrogen gas it is an object of the invention to provide one kind and prepared
A kind of method of oxidation of coal titanium or/and titanium carbide, for the preparation of oxidation of coal titanium and titanium carbide provides new method, to solve existing carbon
Titanium oxide and titanium carbide production technology preparation temperature is high, low production efficiency, it is with high costs a series of problems, such as.
To achieve the above object, present invention employs following technical scheme：
A kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction, comprises the following steps：
Step one：Obtain enough titania powders standby；
Step 2：With addition of iron powder and carbon dust in titania powder, then it is well mixed, the mixed material that will be obtained is used as containing
Titanium reaction raw materials；
Step 3：The titaniferous reaction raw materials of gained are put into reacting furnace, to being continually fed into the mixed of hydrogen and argon gas in reacting furnace
Gas is closed, it is 1200 ~ 1350 DEG C to heat and control reaction in-furnace temperature, and reduction and carbonization treatment is carried out to titaniferous reaction raw materials；
Step 4：Reduction and carbonization completes to be passed through argon gas in backward reacting furnace so that after reduction and carbonization the oxidation of coal titanium of gained or/and
Titanium carbide crude product is cooled to room temperature；
Step 5：The oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after crushing, being finely ground into powder
Leave away except iron tramp therein, obtain oxidation of coal titanium or/and carbonization titanium products.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the step
The titania powder obtained in one, obtains after being sieved by titanium dioxide raw material powder, it is desirable to screening gained titanium dioxide
The grain graininess of powder is 48 mesh ~ 200 mesh.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the dioxy
Change TiO in titanium material powder2Content be more than 95%.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the step
In two, the minimum molar ratio with dosage and titanium dioxide of carbon dust is 1.7：1, the highest of carbon dust is with dosage and titanium dioxide
Molar ratio is 4：1.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the step
In two, iron powder is titania powder and the 5% ~ 10% of carbon dust gross weight with dosage.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the step
Hydrogen used in three and in the mixed gas of argon gas, percent by volume shared by hydrogen is 20% ~ 40%, volume hundred shared by argon gas
Divide than being 60% ~ 80%.
It is above-mentioned with carburetted hydrogen gas reduction to prepare the method for oxidation of coal titanium or/and titanium carbide, preferably, the step
In three, the reaction time of reduction and carbonization is 4.5 ~ 10 hours.
Compared to prior art, the present invention has the advantages that：
1st, the inventive method utilize hydrogen and argon gas mixed gas, titanium dioxide is carried out reduction and carbonization production oxidation of coal titanium or/
With carbonization titanium products, compared with traditional handicraft, processing temperature need to only reach relatively low 1200 ~ 1350 DEG C, and reaction speed faster, drops
Low cost, has reached the purpose of high efficiency, low cost generation oxidation of coal titanium or/and titanium carbide.
2nd, in the inventive method, the reduction characteristic of hydrogen and carbon dust, hydrogen are taken full advantage of in reduction and carbonization processing procedure
There is gas-solid reduction reaction with titanium dioxide first, reduction temperature is low, and reduction efficiency is high, and the presence of carbon dust reduces the oxygen of system
Partial pressure, improves the reproducibility of system, so as to greatly improve the efficiency of reduction, while realizing the carbonization of titanium oxide, carbon
Change temperature low, carbonation rate is fast, saves energy consumption cost.
3rd, the inventive method provides a kind of new technology for the production of oxidation of coal titanium or/and titanium carbide, reduces and is produced into
This, accelerate reaction rate, solve that preparation temperature in existing oxidation of coal titanium and titanium carbide production technology is high, production effect well
Rate is low, it is with high costs a series of problems, such as.
Brief description of the drawings
Fig. 1 is the present invention using titanium dioxide low temperature preparation oxidation of coal titanium or/and the flow chart of titanium carbide method.
Fig. 2 is the XRD thing phasors of products therefrom in the embodiment of the present invention one.
Fig. 3 is the representative fraction of gaseous state phase constituent component in the embodiment of the present invention one and the ratio point of solid-state phase ingredient components
The change curve that number is carried out with reaction.
Specific embodiment
It is directed to oxidation of coal titanium in the prior art and titanium carbide production technology preparation temperature is high, low production efficiency, high cost
High problem, it is the invention provides a kind of new technology for producing oxidation of coal titanium or/and titanium carbide, i.e., a kind of to reduce system with carburetted hydrogen gas
The method of standby oxidation of coal titanium or/and titanium carbide.
It is considered as hydrogen and carbon dust carrys out reduction and carbonization TiO2Powder prepares oxidation of coal titanium or/and titanium carbide, main cause
It is middle utilization pure carbon powder reduction and carbonization high-purity Ti O compared to existing technology2Process for, hydrogen enables to titania powder
There is the titanium oxide that reduction reaction generates low price at more low temperature, and the presence of carbon dust can reduce reaction system
Partial pressure of oxygen, increase reduction potential, while make titanium suboxide be carbonized, promote the carrying out of reduction and carbonization reaction, and help improve
Reaction efficiency.
Therefore, the present invention proposes the new method of a kind of utilization titanium dioxide low temperature preparation oxidation of coal titanium or/and titanium carbide,
The technological process of the method is as shown in figure 1, specifically include following steps：
Step one：Obtain enough titania powders standby.
In the step, acquired titania powder is obtained after preferably being sieved by titanium dioxide raw material powder,
The grain graininess of screening gained titania powder is sought for 48 mesh ~ 200 mesh, is so to be conducive to TiO in subsequent step2Energy
It is enough to be more fully touched reduction and carburizing reagent；And the titanium dioxide raw material powder for specifically using, preferably require wherein
TiO2Content be more than 95%, rutile powder that for example can be using the content of pure titinium dioxide powder or TiO2 more than 95%
Deng as titanium dioxide raw material powder, the control to impurity content is so more beneficial for such that it is able to preferably ensure to obtain pure
Degree oxidation of coal titanium higher or/and carbonization titanium products.
Step 2：With addition of iron powder and carbon dust in titania powder, then it is well mixed, the mixed material that will be obtained is made
It is titaniferous reaction raw materials.
In the step, have certain requirement with dosage to carbon dust, by theory analysis and calculating, carbon dust it is minimum with addition of
Amount will can make the TiO in titania powder2Oxidation of coal titanium is all generated, now the mol ratio of carbon dust and titania powder
It is 1.7：1, the maximum of carbon dust will can make the TiO in titania powder with dosage2All generation titanium carbides, now carbon dust with
The mol ratio of titanium dioxide is 4：1.In addition, adding the catalyst that the effect of iron powder is reacted primarily as reduction and carbonization（Iron unit
Element can promote the carrying out of water gas reaction, so as to reduce oxygen partial pressure）, accelerate the carrying out of reaction, the dosage of iron powder is dioxy
Change the 5% ~ 10% of titanium powder and carbon dust gross weight.
Step 3：The titaniferous reaction raw materials of gained are put into reacting furnace, to being continually fed into hydrogen and argon gas in reacting furnace
Mixed gas, heat and control reaction in-furnace temperature be 1200 ~ 1350 DEG C, titaniferous reaction raw materials are carried out at reduction and carbonization
Reason.
In the step, can be using tube furnace, fixed bed or fluid bed as reacting furnace, to being continually fed into hydrogen in reacting furnace
The mixed gas of gas and argon gas, on the one hand can reach discharge furnace air, play protection against oxidation to titaniferous reaction raw materials
Effect, on the other hand, hydrogen is also the raw material that reduction and carbonization reaction is participated in together with titaniferous reaction raw materials；Reaction in-furnace temperature reaches
During to more than 1200 DEG C, hydrogen is used as the TiO in reducing agent reduction titaniferous reaction raw materials2, react as follows：
H2+nTiO2=TinO2n-1+H2O；
(n-3){H2}+3TinO2n-1=nTi3O5+(n-3)H2O；
H2+2Ti3O5=3Ti2O3+H2O；
H2+Ti2O3=2TiO+H2O。
Wherein, n is the natural number of non-zero.One important function of carbon dust be with product steam reaction, reduce anti-
The partial pressure of oxygen in system is answered, so as to promote hydrogen reducing titanium oxide to react carry out to the right, is reacted as follows：
C + H2O= H2+CO。
The course of reaction of hydrogen and titaniferous reaction raw materials is reaction rate gas-solid reaction faster, therefore its W-response is imitated
Rate is high, course of reaction stablizes easily-controllable；And the TiO or Ti of generation are reacted in titaniferous reaction raw materials2O3Under the high temperature conditions quickly with carbon
There is carburizing reagent, generation oxidation of coal titanium TiC in powderx Oy, react as follows：
TiO+2x C=TiC x O y +xCO；
Or Ti2O3 + (3+2x -2y )C =2TiC x O y + (3-2y)CO；Wherein,x +y=1；
Above-mentioned is incomplete reduction and carbonization reaction, if reaction in-furnace temperature reaches 1250 ~ 1350 DEG C, is matched somebody with somebody in titaniferous reaction raw materials
Plus carbon dust it is sufficient and in the case of the reaction time is sufficiently long, oxidation of coal titanium TiCx OyFollowing reaction then can further occur
Generation titanium carbide：
TiC x O y +2y C = TiC + yCO；Wherein,x +y =1。
In order to the TiO allowed in titaniferous reaction raw materials2Obtain more sufficiently reaction, the hydrogen used in the step
In the mixed gas of argon gas, percent by volume shared by hydrogen needs to reach 20% ~ 40%, and percent by volume shared by argon gas is then
60% ~ 80%, to ensure to possess good, sufficient reduction and carbonization environment in reacting furnace；Meanwhile, maintain carburizing reagent in the step
1200 ~ 1350 DEG C of temperature carries out reaction time of reduction and carbonization and is preferably able to lasting 4.5 ~ 10 hours in stove, to ensure titaniferous
TiO in reaction raw materials2Oxidation of coal titanium or/and titanium carbide are completely converted into as far as possible；Wherein, if reaction in-furnace temperature exists
At 1200 ~ 1250 DEG C, the product of gained is oxidation of coal titanium；If reaction in-furnace temperature is at 1250 ~ 1350 DEG C, in titaniferous reaction raw materials
With addition of carbon dust amount it is sufficient and in the case of the reaction time is sufficiently long, the product of gained is titanium carbide；If reaction in-furnace temperature exists
In 1250 DEG C or more, but titaniferous reaction raw materials with addition of carbon dust amount it is not enough（I.e. the mol ratio of carbon dust and titanium dioxide is 1.7：1
To 4：Between 1）Or in the case of reaction time deficiency, the product of gained is then oxidation of coal titanium and the mixture of titanium carbide.This
Outward, by above-mentioned course of reaction it can also be seen that the main component of tail gas produced by reduction and carbonization process be CO, unreacted it is complete
Full H2, due to being strong reducing property atmosphere, and CO in tail gas2And H2The content of O gases is very low, therefore tail gas can be subject to
Recycle；And mode is recycled as preferred, tail gas can be used to carry out separating treatment obtain hydrogen and an oxidation
Carbon gas, wherein fuel of the isolated CO gas as heating reaction furnace, and isolated hydrogen is then
It is used to rejoin participation reaction in reacting furnace, help reduces the consumption of energy consumption and hydrogen feed, so as to further drop
Low production cost.
Step 4：Reduction and carbonization completes to be passed through argon gas in backward reacting furnace so that the oxidation of coal titanium of gained after reduction and carbonization
Or/and titanium carbide crude product is cooled to room temperature.
In reacting furnace by the product after reduction and carbonization be oxidation of coal titanium or/and titanium carbide crude product containing iron powder, the step
Suddenly it is made to treat subsequent treatment after being cooled under argon gas protection environment, in case being oxidized in its cooling procedure.
Step 5：The oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic is carried out after crushing, being finely ground into powder
Choosing separates removal iron tramp therein, obtains oxidation of coal titanium or/and carbonization titanium products.
In the step, magnetic separation is first carried out by the oxidation of coal titanium or/and titanium carbide crude product after cooling be broken, after fine grinding, can be with
So that iron powder impurity therein is separated by magnetic, and the magnetic separation clout of gained is then pure oxidation of coal titanium or/and titanium carbide product
Product.
Be can see by above-mentioned handling process, the inventive method is using hydrogen and carbon reducing agent carbonization TiO2It is prepared by powder
Oxidation of coal titanium or/and titanium carbide, processing temperature need to only reach relatively low 1200 ~ 1350 DEG C, and this is the reproducibility ratio due to hydrogen
The reproducibility of carbon dust is strong, so hydrogen can occur gas-solid reduction reaction, reduction effect with titanium dioxide first at a lower temperature
Rate is high, while the vapor produced after the carbon dust fully mixed with titanium dioxide and hydrogen reducing occurs water gas reaction, reduces
Partial pressure of oxygen in reacting furnace, promotes the further reduction of titanium oxide, and well mixed carbon dust also greatly improves carbonization
Efficiency, carbonation rate is fast, realizes the purpose of reduction and carbonization titanium oxide at a lower temperature, saves energy consumption cost；In addition
Main Ingredients and Appearance in tail gas product is CO and H2, recoverable can help further reduce production cost.It can be seen that, this hair
The bright method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction reduces production cost, accelerates production reaction rate,
Preparation temperature in existing oxidation of coal titanium and titanium carbide production technology high, low production efficiency, with high costs etc. one is solved well
Series of problems.
The present invention is described in further detail with instantiation below in conjunction with the accompanying drawings.
Example one：
The present embodiment uses TiO2Content be 96% rutile as titanium dioxide raw material powder, prepare oxidation of coal titanium or/and carbon
Change titanium, comprise the following steps that：
（1）By TiO2Content is that 96% rutile powder is sieved, and obtains enough titania powders, it is desirable to sieve institute
The grain graininess for obtaining titania powder is 48 mesh ~ 200 mesh.
（2）With addition of appropriate carbon dust in the titania powder for obtaining so that carbon dust and titania powder mole
Than being 1.7：1, while adding a certain amount of iron powder again, the addition of iron powder is carbon dust and titania powder gross weight
8.2%, as titaniferous reaction mass after titaniferous material is mixed.
（3）The titaniferous reaction raw materials of gained are put into MgO crucibles, are then placed in tube furnace, and be continually fed into argon gas：
Hydrogen is 60%：40% mixed gas, heat and control tubular type in-furnace temperature to carry out 4.5 hours of reduction and carbonization for 1200 DEG C,
Reduction and carbonization treatment is carried out to titaniferous reaction raw materials.
（4）Reduction and carbonization completes to be passed through argon gas in backward tube furnace, by the oxidation of coal titanium or/and carbon of gained after reduction and carbonization
Change titanium crude product and be cooled to room temperature.Mutually detected through thing, the thing of the present embodiment gained oxidation of coal titanium or/and titanium carbide crude product mutually detects knot
Fruit is as shown in Fig. 2 in fig. 2, label 4 represents Ti2O3Thing phase, label 5 represents TiC x O y Thing phase, it can thus be concluded that knowing this implementation
The main thing of product is mutually oxidation of coal titanium in example.
（5）The oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after crushing, being finely ground into powder
Leave away except iron tramp therein.
Mutually detected through thing, the ratio of the representative fraction of gaseous state phase constituent component and solid-state phase ingredient components point in the present embodiment
Number is with the change curve that carries out of reaction as shown in figure 3, from the figure 3, it may be seen that the present embodiment products therefrom is oxidation of coal titanium, containing
Minimal amount of Ti2O3, product is mainly CO and H in gas phase2, with value very high.Additionally, the present embodiment is also to reduction
The tail gas that carbonisation is produced has carried out sections of a city close to the city wall detection, and its result is consistent with result shown in Fig. 3, and primary product is CO and H2。
Example two：
The present embodiment uses TiO2Content be 99% titania powder as titanium dioxide raw material powder, prepare oxidation of coal titanium
Or/and titanium carbide, comprise the following steps that：
（1）By TiO2Content is that 99% titania powder is sieved, and obtains enough titania powders, it is desirable to sieve
The grain graininess of gained titania powder is 48 mesh ~ 200 mesh.
（2）With addition of appropriate carbon dust in the titania powder for obtaining so that carbon dust and titania powder mole
Than being 3：1, while adding a certain amount of iron powder again, the addition of iron powder is the 8.2% of carbon dust and titania powder gross weight,
As titaniferous reaction mass after titaniferous material is mixed.
（3）The titaniferous reaction raw materials of gained are put into MgO crucibles, are then placed in tube furnace, and be continually fed into argon gas：
Hydrogen is 80%：20% mixed gas, heat and control tubular type in-furnace temperature to be carried out 10 hours of reduction and carbonization for 1250 DEG C, right
Titaniferous reaction raw materials carry out reduction and carbonization treatment.
（4）Reduction and carbonization completes to be passed through argon gas in backward tube furnace, by the oxidation of coal titanium or/and carbon of gained after reduction and carbonization
Change titanium crude product and be cooled to room temperature.Mutually detected through thing, the main thing of the present embodiment gained oxidation of coal titanium or/and titanium carbide crude product is mutually
Oxidation of coal titanium, it can thus be concluded that the main thing for knowing product in the present embodiment is mutually oxidation of coal titanium.
（5）The oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after crushing, being finely ground into powder
Leave away except iron tramp therein.
Additionally, also having carried out embodiment twice, respectively embodiment three and example IV using the inventive method.Each time real
The major parameter and products therefrom for applying example are as shown in the table.
Be can see by above-mentioned each embodiment, the present invention prepares the side of oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction
Method, can prepare oxidation of coal titanium or/and titanium carbide under the conditions of lower temperature, significantly be dropped on energy consumption cost
It is low, preparation temperature in existing oxidation of coal titanium and titanium carbide production technology high, low production efficiency, with high costs etc. are solved well
Problem, and the method be applied to linking Producing Titanium Dioxide flow, so as to produce added value it is higher containing titanium products, with fine
Industrial application value.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, it all should cover at this
In the middle of the right of invention.
Claims (7)
1. a kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction, it is characterised in that comprise the following steps：
Step one：Obtain enough titania powders standby；
Step 2：With addition of iron powder and carbon dust in titania powder, then it is well mixed, the mixed material that will be obtained is used as containing
Titanium reaction raw materials；
Step 3：The titaniferous reaction raw materials of gained are put into reacting furnace, to being continually fed into the mixed of hydrogen and argon gas in reacting furnace
Gas is closed, it is 1200 ~ 1350 DEG C to heat and control reaction in-furnace temperature, and reduction and carbonization treatment is carried out to titaniferous reaction raw materials；
Step 4：Reduction and carbonization completes to be passed through argon gas in backward reacting furnace so that after reduction and carbonization the oxidation of coal titanium of gained or/and
Titanium carbide crude product is cooled to room temperature；
Step 5：The oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after crushing, being finely ground into powder
Leave away except iron tramp therein, obtain oxidation of coal titanium or/and carbonization titanium products.
2. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 1, it is characterised in that institute
The titania powder obtained in step one is stated, is obtained after being sieved by titanium dioxide raw material powder, it is desirable to screening gained two
The grain graininess of titanium dioxide powder is 48 mesh ~ 200 mesh.
3. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 2, it is characterised in that institute
State TiO in titanium dioxide raw material powder2Content be more than 95%.
4. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 1, it is characterised in that institute
State in step 2, the minimum molar ratio with dosage and titanium dioxide of carbon dust is 1.7：1, the highest of carbon dust matches somebody with somebody dosage and dioxy
The molar ratio for changing titanium is 4：1.
5. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 1, it is characterised in that institute
State in step 2, iron powder is titania powder and the 5% ~ 10% of carbon dust gross weight with dosage.
6. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 1, it is characterised in that institute
State in the mixed gas of the hydrogen and argon gas used in step 3, percent by volume shared by hydrogen is 20% ~ 40%, shared by argon gas
Percent by volume is 60% ~ 80%.
7. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as claimed in claim 1, it is characterised in that institute
State in step 3, the reaction time of reduction and carbonization is 4.5 ~ 10 hours.
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| CN107737943A (en) * | 2017-11-03 | 2018-02-27 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN107758669A (en) * | 2017-11-30 | 2018-03-06 | 重庆大学 | A kind of method that propyl alcohol reduction prepares Molybdenum carbide powders |
| WO2020147464A1 (en) * | 2019-01-14 | 2020-07-23 | 浙江海虹控股集团有限公司 | Method for preparing titanium-containing composite anode at low temperature |
| CN114436262A (en) * | 2022-03-24 | 2022-05-06 | 昆明理工大学 | Method for preparing titanium carbide |
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| CN101386407A (en) * | 2008-10-23 | 2009-03-18 | 武汉工程大学 | Method for preparing nano carbon tube/titanium carbide(nitride) composite powder |
| CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101386407A (en) * | 2008-10-23 | 2009-03-18 | 武汉工程大学 | Method for preparing nano carbon tube/titanium carbide(nitride) composite powder |
| CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107737943A (en) * | 2017-11-03 | 2018-02-27 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN107737943B (en) * | 2017-11-03 | 2019-08-02 | 重庆大学 | A kind of method that Reduction of methanol prepares tungsten carbide or/and tungsten powder |
| CN107758669A (en) * | 2017-11-30 | 2018-03-06 | 重庆大学 | A kind of method that propyl alcohol reduction prepares Molybdenum carbide powders |
| CN107758669B (en) * | 2017-11-30 | 2019-11-08 | 重庆大学 | A kind of method that propyl alcohol reduction prepares Molybdenum carbide powders |
| WO2020147464A1 (en) * | 2019-01-14 | 2020-07-23 | 浙江海虹控股集团有限公司 | Method for preparing titanium-containing composite anode at low temperature |
| CN114436262A (en) * | 2022-03-24 | 2022-05-06 | 昆明理工大学 | Method for preparing titanium carbide |
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