CN106744960B - A method of oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction - Google Patents
A method of oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction Download PDFInfo
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Abstract
The present invention provides a kind of methods for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, this method is using pure titinium dioxide or rutile as initial feed, select 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 lower 1200 ~ 1350 DEG C, gas-solid reduction reaction occurs for hydrogen and titaniferous materials during preparing oxidation of coal titanium or/and titanium carbide, reduction efficiency is high, reduction rate is fast, water gas reaction occurs for the vapor generated after the carbon dust and hydrogen reducing that mix well with raw material, reduce the partial pressure of oxygen in material bed, to promote the progress of titanium oxide reduction reaction, uniformly 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, section Energy consumption cost is saved, the problems such as preparation temperature is high, production efficiency is low, with high costs in the existing oxidation of coal titanium of very good solution and titanium carbide production technology.
Description
Technical field
The present invention relates to chemical metallurgy technical fields, 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 technique
Titanium carbide is a kind of material high with fusing point, the good characteristics such as hardness is high, chemical stability is good, in industrial production
It is usually used to manufacture cermet, heat-resisting alloy and hard alloy in the process, these products are in aerospace, coating material etc.
High-tech area, which has a very wide range of applications, (can refer to document " Liu Yang, Zeng Lingke；Chinese pottery, 2002,38；7~10
Page ").
At present both at home and abroad there are many kinds of the methods of synthesizing titanium carbide, what is industrially mainly used 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 " report
TiO is restored using carbon black2Powder obtains titanium carbide powder.But this method there are the problem of be also apparent from: because of reactant
Exist with the particle of dispersion, reacts the degree of progress by 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 wider particle size distribution, and ball milling is needed to process；Reaction time is longer, about at 10 ~ 20 hours, instead
Keep the powder of synthesis usually not pure enough due to being influenced by diffusion gradient in answering；It is also very high to react the temperature needed, about
1700 ~ 2100 DEG C, comprehensive energy consumption is very big.
Document " Feng Chengjian, Zhang Jianshu；Mineral products comprehensive utilization, 1997,6；34-41 pages " report contained using high-purity carbon reducing agent
Titanium blast furnace slag (TiO2: 22% ~ 23%) produce titanium carbide.There is also some problems for this method: the temperature for reacting needs is higher, about
It is 1600 DEG C；Since TiC is a kind of high-temperature product, in carbonation reaction, the TiC of generation is in that the solia particle of relatively dispersion is outstanding
It floats in slag liquid, increases viscosity, prevent the reunion of TiC particle, so the TiC granularity obtained after high temperature cabonization is too thin, and
And TiC particle easily forms abundance zone around carbon granules or iron shot, general milling method can not make mineral reach effective monomer solution
From to cause later purification TiC more difficult.
Past many decades extract titanium technique by the electrolysis method of medium of fused salt to reduce the cost of titanium smelting process
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, it is molten that 2007,438:243-246 " reports a kind of new carbon thermal reduction-
Salt electroextraction titanium technique (USTB technique) proposes novel soluble electrolytic anode material oxidation of coal titanium (TiC x O y ,x+y=
1).It facts have proved that this technique is a kind of very promising method in numerous Titanium new preparation processes.But ideal electrolytic anode
Preparation be restrictive condition that the technique further develops.In prior art process, TiC is prepared x O y Method be carbon heat also
Former method utilizes the TiO of carbon dust direct-reduction high-purity2Powder, the reaction process need to carry out reaction condition stringent control
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 conclusion the preparation method of current oxidation of coal titanium or/and titanium carbide, is on the one hand to utilize high pure raw material, it is this kind of
The available high-purity product of method, saves subsequent purification process, but cost of material is high, and process energy consumption is greatly to make
It is greatly improved at production cost；It on the one hand is to utilize TiO2The lower titaniferous materials of grade, although the temperature that such methods need
It is relatively low, but subsequent purification process is sufficiently complex, process flow is long, and production efficiency is lower.Therefore, it needs a kind of new
Low cost, low energy consumption, efficient oxidation of coal titanium or/and titanium carbide preparation process.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, the purpose of the present invention is to provide one kind with carburetted hydrogen gas reduction preparation
The method of oxidation of coal titanium or/and titanium carbide provides a kind of new method for the preparation of oxidation of coal titanium and titanium carbide, to solve existing carbon
A series of problems, such as titanium oxide and titanium carbide production technology preparation temperature are high, production efficiency is low, with high costs.
To achieve the above object, present invention employs the following technical solutions:
A method of oxidation of coal titanium or/and titanium carbide being prepared with carburetted hydrogen gas reduction, is included the following steps:
Step 1: it is spare that enough titania powders are obtained；
Step 2: with addition of iron powder and carbon dust in titania powder, being then uniformly mixed, and obtained mixed material is made
For titaniferous reaction raw materials；
Step 3: resulting titaniferous reaction raw materials are put into reacting furnace, hydrogen and argon gas are continually fed into reacting furnace
Mixed gas, heat and control reaction in-furnace temperature be 1200 ~ 1350 DEG C, to titaniferous reaction raw materials carry out reduction and carbonization at
Reason；
Step 4: reduction and carbonization is passed through argon gas into reacting furnace after completing, so that resulting oxidation of coal titanium after reduction and carbonization
Or/and titanium carbide crude product is cooled to room temperature；
Step 5: oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, carries out magnetic after being crushed, being finely ground into powder
Choosing separation removes iron tramp therein, obtains oxidation of coal titanium or/and carbonization titanium products.
It is above-mentioned to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the step
The titania powder obtained in one obtains after being sieved by titanium dioxide raw material powder, it is desirable that screening gained titanium dioxide
The grain graininess of powder is 48 mesh ~ 200 mesh.
It is above-mentioned to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the dioxy
Change TiO in titanium material powder2Content be greater than 95%.
It is above-mentioned to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the step
In two, the minimum molar ratio with dosage and titanium dioxide of carbon dust is 1.7:1, and the highest of carbon dust is with dosage and titanium dioxide
Molar ratio is 4:1.
It is above-mentioned to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the step
In two, iron powder is titania powder and the 5% ~ 10% of carbon dust total weight with dosage.
It is above-mentioned to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the step
In the mixed gas of hydrogen used in three and 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 to be prepared in the method for oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, preferably, the step
In three, the reaction time of reduction and carbonization is 4.5 ~ 10 hours.
Compared with the prior art, the invention has the following beneficial effects:
1, the method for the present invention utilizes hydrogen and argon gas mixed gas, carries out reduction and carbonization to titanium dioxide and produces oxidation of coal titanium
Or/and carbonization titanium products, compared with traditional handicraft, processing temperature need to only reach lower 1200 ~ 1350 DEG C, and reaction speed is more
Fastly, it reduces costs, has achieved the purpose that high efficiency, low cost generates oxidation of coal titanium or/and titanium carbide.
2, in the method for the present invention, the reduction characteristic of hydrogen and carbon dust, hydrogen are taken full advantage of in reduction and carbonization treatment process
Gas-solid reduction reaction occurs 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, to greatly improve the efficiency of reduction, while realizing the carbonization of titanium oxide, carbon
Change temperature is low, and carbonation rate is fast, saves energy consumption cost.
3, the method for the present invention provides a kind of new process for the production of oxidation of coal titanium or/and titanium carbide, reduces and is produced into
This, accelerate reaction rate, preparation temperature is high in the existing oxidation of coal titanium of very good solution and titanium carbide production technology, production effect
A series of problems, such as rate is low, with high costs.
Detailed description of the invention
Fig. 1 is that the present invention utilizes titanium dioxide low temperature preparation oxidation of coal titanium or/and the flow chart of titanium carbide method.
Fig. 2 is the XRD object phasor of products therefrom in the embodiment of the present invention one.
Fig. 3 is the ratio of the representative fraction of gaseous state phase constituent component and solid-state phase ingredient components point in the embodiment of the present invention one
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 height, production efficiency is low, at high cost
High problem, it is the present invention provides a kind of new process for producing oxidation of coal titanium or/and titanium carbide, i.e., a kind of with carburetted hydrogen gas reduction system
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 to utilize pure carbon powder reduction and carbonization high-purity Ti O compared to the prior art2Process for, hydrogen enables to titania powder
The titanium oxide of low price is generated in more low at a temperature of generation reduction reaction, and the presence of carbon dust can reduce reaction system
Partial pressure of oxygen, increase reduction potential, while titanium suboxide being made to be carbonized, promote the progress of reduction and carbonization reaction, and help to improve
Reaction efficiency.
Therefore, the invention proposes a kind of new method using titanium dioxide low temperature preparation oxidation of coal titanium or/and titanium carbide,
The process flow of this method is as shown in Figure 1, specifically comprise the following steps:
Step 1: it is spare that enough titania powders are obtained.
In the step, acquired titania powder is obtained after preferably being sieved by titanium dioxide raw material powder,
The grain graininess for seeking screening gained titania powder is 48 mesh ~ 200 mesh, is to be conducive to TiO in subsequent step in this way2Energy
It is enough more fully to be contacted reduction and carburizing reagent；And the titanium dioxide raw material powder specifically used, it preferably requires wherein
TiO2Content be greater than 95%, such as 95% rutile powder can be greater than using the content of pure titinium dioxide powder or TiO2
Deng be used as titanium dioxide raw material powder, be more advantageous to the control to impurity content in this way, it is pure so as to preferably guarantee to obtain
Spend higher oxidation of coal titanium or/and carbonization titanium products.
Step 2: with addition of iron powder and carbon dust in titania powder, being then uniformly mixed, and obtained mixed material is made
For 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 wants that the TiO in titania powder can be made2Oxidation of coal titanium is all generated, at this time the molar ratio of carbon dust and titania powder
Maximum for 1.7:1, carbon dust with dosage wants that the TiO in titania powder can be made2All generate titanium carbides, at this time carbon dust with
The molar ratio of titanium dioxide is 4:1.In addition, catalyst (the iron member that the effect that iron powder is added is reacted primarily as reduction and carbonization
Element can promote the progress of water gas reaction, to reduce oxygen partial pressure), accelerate the progress of reaction, the dosage of iron powder is dioxy
Change the 5% ~ 10% of titanium powder and carbon dust total weight.
Step 3: resulting titaniferous reaction raw materials are put into reacting furnace, hydrogen and argon gas are continually fed into reacting furnace
Mixed gas, heat and control reaction in-furnace temperature be 1200 ~ 1350 DEG C, to titaniferous reaction raw materials carry out reduction and carbonization at
Reason.
In the step, hydrogen can be continually fed into reacting furnace using tube furnace, fixed bed or fluidized bed as reacting furnace
On the one hand the mixed gas of gas and argon gas can achieve discharge furnace air, play protection against oxidation to titaniferous reaction raw materials
Effect, on the other hand, hydrogen are also the raw material that reduction and carbonization reaction is participated in together with titaniferous reaction raw materials；Reaction in-furnace temperature reaches
When to 1200 DEG C or more, hydrogen is as the TiO in reducing agent reduction titaniferous reaction raw materials2, it reacts 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 reaction product steam reaction, reduce anti-
The partial pressure of oxygen in system is answered, so that the reaction of hydrogen reducing titanium oxide be promoted to carry out to the right, is reacted as follows:
C + H2O= H2+CO。
The reaction process of hydrogen and titaniferous reaction raw materials is the faster gas-solid reaction of reaction rate, therefore its W-response is imitated
Rate height, reaction process are stablized easily-controllable；And the TiO or Ti of generation are reacted in titaniferous reaction raw materials2O3Under the high temperature conditions quickly with carbon
Carburizing reagent occurs for powder, generates oxidation of coal titanium TiCxOy, it reacts as follows:
TiO+2xC=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, titaniferous reaction raw materials
In with addition of under carbon dust is sufficient and reaction time sufficiently long situation, oxidation of coal titanium TiCxOyThen can further it occur following anti-
Titanium carbide should be generated:
TiC x O y +2yC = TiC + yCO；Wherein,x+y=1。
In order to the TiO allowed in titaniferous reaction raw materials2It obtains more adequately reacting, 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 guarantee to have in reacting furnace good, sufficient reduction and carbonization environment；Meanwhile carburizing reagent is maintained in the step
The reaction time that 1200 ~ 1350 DEG C of temperature carries out reduction and carbonization in furnace is preferably able to lasting 4.5 ~ 10 hours, to guarantee titaniferous
TiO in reaction raw materials2It is completely converted into oxidation of coal titanium or/and titanium carbide as far as possible；Wherein, if reaction in-furnace temperature exists
At 1200 ~ 1250 DEG C, resulting product is oxidation of coal titanium；If reacting in-furnace temperature in 1250 ~ 1350 DEG C, titaniferous reaction raw materials
With addition of under carbon dust amount is sufficient and reaction time sufficiently long situation, resulting product is titanium carbide；If reaction in-furnace temperature exists
1250 DEG C or more, but in titaniferous reaction raw materials with addition of carbon dust amount insufficient (i.e. the molar ratio of carbon dust and titanium dioxide is in 1.7:1
To between 4:1) or reaction time insufficient situation under, resulting product is then the mixture of oxidation of coal titanium and titanium carbide.This
Outside, by above-mentioned reaction process it can also be seen that the main component of tail gas caused by reduction and carbonization process is that CO, unreacted are complete
Full H2, due to being strong reducing property atmosphere, and CO in tail gas2And H2The content of O gas is very low, therefore can be subject to tail gas
It recycles；And mode is recycled as preferred, tail gas can be obtained into hydrogen and an oxidation to carry out separating treatment
Carbon gas, wherein isolated CO gas is to the fuel as heating reaction furnace, and isolated hydrogen is then
Reaction is participated in reacting furnace to rejoin, and the consumption for reducing production energy consumption and hydrogen feed is helped, to further drop
Low production cost.
Step 4: reduction and carbonization is passed through argon gas into reacting furnace after completing, so that resulting oxidation of coal titanium after reduction and carbonization
Or/and titanium carbide crude product is cooled to room temperature.
Product in reacting furnace after reduction and carbonization is oxidation of coal titanium or/and titanium carbide crude product containing iron powder, the step
Suddenly to subsequent processing after making it cool under argon gas protection environment, to prevent being oxidized in its cooling procedure.
Step 5: oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, carries out magnetic after being crushed, being finely ground into powder
Choosing separation removes iron tramp therein, obtains oxidation of coal titanium or/and carbonization titanium products.
In the step, oxidation of coal titanium after cooling or/and titanium carbide crude product are first subjected to magnetic separation after broken, fine grinding, it can be with
So that iron powder impurity therein is separated by magnetic, and resulting magnetic separation clout is then that pure oxidation of coal titanium or/and titanium carbide produce
Product.
It can see by above-mentioned process flow, the method for the present invention is using hydrogen and carbon reducing agent carbonization TiO2Powder preparation
Oxidation of coal titanium or/and titanium carbide, processing temperature need to only reach lower 1200 ~ 1350 DEG C, this is because the reproducibility ratio of hydrogen
The reproducibility of carbon dust is strong, so gas-solid reduction reaction, reduction effect can occur with titanium dioxide first at a lower temperature for hydrogen
Rate is high, while water gas reaction occurs for the vapor generated after the carbon dust and hydrogen reducing mixed well with titanium dioxide, reduces
Partial pressure of oxygen in reacting furnace, promotes the further reduction of titanium oxide, uniformly 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；Furthermore
Main ingredient in tail gas product is CO and H2, recoverable can help further reduce production cost.As it can be seen that this hair
It is bright to prepare oxidation of coal titanium or/and the method for titanium carbide with carburetted hydrogen gas reduction and reduce production cost, accelerate production reaction rate,
Preparation temperature is high in the existing oxidation of coal titanium of very good solution and titanium carbide production technology, production efficiency is low, with high costs etc. one
Series of problems.
The present invention is described in further detail with specific example with reference to the accompanying drawing.
Example one:
The present embodiment uses TiO2The rutile that content is 96% as titanium dioxide raw material powder, prepare oxidation of coal titanium or/
And titanium carbide, the specific steps are as follows:
(1) by TiO2The rutile powder that content is 96% is sieved, and enough titania powders are obtained, it is desirable that sieve
The grain graininess of titania powder obtained by point is 48 mesh ~ 200 mesh.
(2) with addition of suitable carbon dust in obtained titania powder, so that mole of carbon dust and titania powder
Than for 1.7:1, while a certain amount of iron powder is added again, the additive amount of iron powder is carbon dust and titania powder total weight
8.2%, titaniferous reaction mass is used as after titaniferous material is mixed.
(3) resulting titaniferous reaction raw materials are put into MgO crucible, are then placed in tube furnace, and be continually fed into argon gas:
Hydrogen is the mixed gas of 60%:40%, and heating and controlling tubular type in-furnace temperature is 1200 DEG C of 4.5 hours of progress reduction and carbonization,
Reduction and carbonization processing is carried out to titaniferous reaction raw materials.
(4) reduction and carbonization is passed through argon gas into tube furnace after completing, by oxidation of coal titanium resulting after reduction and carbonization or/and carbon
Change titanium crude product to be cooled to room temperature.It is mutually detected through object, the object of oxidation of coal titanium obtained by the present embodiment or/and titanium carbide crude product mutually detects knot
For fruit as shown in Fig. 2, in Fig. 2, label 4 indicates Ti2O3Object phase, label 5 indicate TiC x O y Object phase, it can thus be concluded that the present embodiment
The main object of middle product is mutually oxidation of coal titanium.
(5) oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after being crushed, being finely ground into powder
It leaves away except iron tramp therein.
It is mutually detected through object, the ratio of the representative fraction of gaseous state phase constituent component and solid-state phase ingredient components point in the present embodiment
Number with reaction carry out change curves as shown in figure 3, from the figure 3, it may be seen that the present embodiment products therefrom be oxidation of coal titanium, contain
Minimal amount of Ti2O3, product is mainly CO and H in gas phase2, there is very high utility value.In addition, the present embodiment is also to reduction
The tail gas that carbonisation generates has carried out sections of a city close to the city wall detection, and result is consistent with result shown in Fig. 3, and primary product is CO and H2。
Example two:
The present embodiment uses TiO2The titania powder that content is 99% prepares carbon oxygen as titanium dioxide raw material powder
Change titanium or/and titanium carbide, the specific steps are as follows:
(1) by TiO2The titania powder that content is 99% is sieved, and enough titania powders are obtained, it is desirable that
The grain graininess of screening gained titania powder is 48 mesh ~ 200 mesh.
(2) with addition of suitable carbon dust in obtained titania powder, so that mole of carbon dust and titania powder
Than for 3:1, while a certain amount of iron powder is added again, the additive amount of iron powder is the 8.2% of carbon dust and titania powder total weight,
Titaniferous reaction mass is used as after titaniferous material is mixed.
(3) resulting titaniferous reaction raw materials are put into MgO crucible, are then placed in tube furnace, and be continually fed into argon gas:
Hydrogen is the mixed gas of 80%:20%, and heating and controlling tubular type in-furnace temperature is 1250 DEG C of 10 hours of progress reduction and carbonization, right
Titaniferous reaction raw materials carry out reduction and carbonization processing.
(4) reduction and carbonization is passed through argon gas into tube furnace after completing, by oxidation of coal titanium resulting after reduction and carbonization or/and carbon
Change titanium crude product to be cooled to room temperature.It is mutually detected through object, the main object of oxidation of coal titanium obtained by the present embodiment or/and titanium carbide crude product is mutually
Oxidation of coal titanium, it can thus be concluded that the main object of product is mutually oxidation of coal titanium in the present embodiment.
(5) oxidation of coal titanium or/and titanium carbide crude product after cooling are taken out, magnetic separation point is carried out after being crushed, being finely ground into powder
It leaves away except iron tramp therein.
In addition, also having carried out embodiment twice, respectively embodiment three and example IV using the method for the present invention.Each time real
Major parameter and the products therefrom for applying example are as shown in the table.
It can see by above-mentioned each embodiment, the present invention prepares oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction
Method, oxidation of coal titanium or/and titanium carbide can be prepared under the conditions of lower temperature, be able to substantially on energy consumption cost
Reduction, preparation temperature is high in the existing oxidation of coal titanium of very good solution and titanium carbide production technology, production efficiency is low, at high cost
The problems such as high, and this method is suitable for linking Producing Titanium Dioxide process, and to produce, added value is higher to contain titanium products, has
Good industrial application value.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (5)
1. a kind of method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction, which comprises the steps of:
Step 1: it is spare that enough titania powders are obtained；
Step 2: with addition of iron powder and carbon dust in titania powder, being then uniformly mixed, using obtained mixed material as containing
Titanium reaction raw materials；Wherein, the minimum molar ratio with dosage and titanium dioxide of carbon dust is 1.7:1, and the highest of carbon dust matches dosage
Molar ratio with titanium dioxide is 4:1；Iron powder is titania powder and the 5% ~ 10% of carbon dust total weight with dosage；
Step 3: resulting titaniferous reaction raw materials are put into reacting furnace, and the mixed of hydrogen and argon gas is continually fed into reacting furnace
Gas is closed, heating and controlling reaction in-furnace temperature is 1200 ~ 1350 DEG C, carries out reduction and carbonization processing to titaniferous reaction raw materials；
Step 4: reduction and carbonization complete after argon gas is passed through into reacting furnace so that after reduction and carbonization resulting oxidation of coal titanium or/and
Titanium carbide crude product is cooled to room temperature；
Step 5: taking out oxidation of coal titanium or/and titanium carbide crude product after cooling, and magnetic separation point is carried out after being crushed, being finely ground into powder
It leaves away except iron tramp therein, obtains 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 described in claim 1, which is characterized in that institute
The titania powder obtained in step 1 is stated, is obtained after being sieved by titanium dioxide raw material powder, it is desirable that 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, which is characterized in that institute
State TiO in titanium dioxide raw material powder2Content be greater than 95%.
4. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as described in claim 1, which is characterized in that institute
In the mixed gas for stating hydrogen used in step 3 and argon gas, percent by volume shared by hydrogen is 20% ~ 40%, shared by argon gas
Percent by volume is 60% ~ 80%.
5. the method for preparing oxidation of coal titanium or/and titanium carbide with carburetted hydrogen gas reduction as described in claim 1, which is characterized in that institute
It states in step 3, the reaction time of reduction and carbonization is 4.5 ~ 10 hours.
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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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| 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 |
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