CN109110804A - Sub- titanium oxide of high-purity Magn é li phase and preparation method thereof - Google Patents
Sub- titanium oxide of high-purity Magn é li phase and preparation method thereof Download PDFInfo
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- CN109110804A CN109110804A CN201811331281.3A CN201811331281A CN109110804A CN 109110804 A CN109110804 A CN 109110804A CN 201811331281 A CN201811331281 A CN 201811331281A CN 109110804 A CN109110804 A CN 109110804A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/043—Titanium sub-oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to field of inorganic materials, and in particular to the preparation method of the sub- titanium oxide of high-purity Magn é li phase.The preparation method of the sub- titanium oxide of high-purity Magn é li phase, step are as follows: by TiO2With binder mixed pelletization, obtaining diameter is 2~5mm particle A；Particle A and reducing agent are pressed into one layer of reducing agent, one layer of particle A, are staggeredly put into reactor, and top layer is reducing agent；A layers of particle are all made of monolayer of particles A covering；In addition to top layer's reducing agent, every layer of reducing agent cladding thickness >=2cm；Cladding thickness >=10cm of top layer's reducing agent；Reducing agent granularity≤74 μm；Reactor is restored into 30~60min at 1250~1450 DEG C, after take out reactor cool down in an inert atmosphere, obtain reduzate；By reduzate screening, cleaning, the sub- titanium oxide of high-purity Magn é li phase is obtained.The sub- titanium oxide of high-purity Magn é li phase obtained, purity is high, residual carbon content are low.
Description
Technical field
The present invention relates to field of inorganic materials, and in particular to sub- titanium oxide of high-purity Magn é li phase and preparation method thereof.
Background technique
In recent years, the sub- titanium oxide of Magn é li phase is in inert electrode, fuel cell, lithium battery, photocatalysis and conductive additive
Etc. application there are many reports, become one of the research hotspot of domestic and international titanium functional material.Magn é li phase oxidation titanium master
There are three kinds of high temperature reduction method, laser ablation method and collosol and gel-sintering process preparation processes.The preparation of Magn é li phase oxidation titanium
Mainly with TiO2For raw material, current preparation method is long there are the reaction process time, and reaction harsh to reaction atmosphere requirement produces
The disadvantages of object physico-chemical property is difficult to control.
Carbothermic method due to its simple process, it is at low cost, low for equipment requirements the advantages that be widely used in material system
Standby field.
Application No. is 2017101201355 Chinese patents to disclose a kind of graphite-titanium suboxide composite material
Preparation method.This method is mixed with titanium dioxide using graphite powder, and by graphite powder uniform fold on mixed material surface, into
The reaction of row high temperature reduction.Although this method provides a kind of means reacted in air atmosphere, the production of this method preparation
Object remains as graphite-titanium suboxide composite material, and remaining graphite or coal dust difficulty and reduzate are effective in reduzate
Separation cannot prepare the sub- titanium oxide of high-purity Magn é li phase, limit its application the expansion in field.
Therefore, the preparation work that the sub- titanium oxide of high-purity Magn é li phase is prepared with one completely new carbothermic method of exploitation is explored
Skill route is very necessary.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of carbothermic method to prepare the sub- titanium oxide of high-purity Magn é li phase
Method.
The preparation method of the sub- titanium oxide of high-purity Magn é li phase, sequentially includes the following steps:
A, by TiO2It mixes, pelletizes by weight 1:0.05~0.1 with binder, drying, obtaining diameter is 2~5mm's
Particle A；
B, particle A and reducing agent are pressed into one layer of reducing agent, one layer of particle A, are staggeredly put into reactor, and top layer covers
Layer is reducing agent；Wherein, reducing agent is graphite powder or coal dust；A layers of particle are all made of monolayer of particles A covering, and cladding thickness is
The diameter of particle A；In addition to top layer's reducing agent, cladding thickness >=2cm of every layer of reducing agent；The cladding thickness of top layer's reducing agent
≥10cm；Granularity≤74 μm of reducing agent；
C, reactor is placed in 30~60min of reduction at 1250~1450 DEG C, reactor is taken out after reduction in inertia
It is cooling in atmosphere, obtain reduzate；
D, reduzate is sieved, obtains the sub- titanium oxide of granular Magn é li phase and reducing agent；
F, the remaining reducing agent of the sub- titania surface of granular Magn é li phase is cleaned, the sub- oxidation of high-purity Magn é li phase is obtained
Titanium.
Preferably, in step a, binder is polyvinyl alcohol.
Preferably, in step a: the diameter of particle A is 2.5~5mm；It is furthermore preferred that the diameter of particle A is 2.5mm.
Preferably, in step a: TiO2Purity is 99% or more.
Preferably, in step b, every layer of reducing agent cladding thickness is 2.2~3cm, and the cladding thickness of top layer's reducing agent
For 12~15cm；Preferably, every layer of reducing agent cladding thickness is 2.2cm, and the cladding thickness of top layer's reducing agent is 12cm.
Preferably, in step b, reactor is graphiote reactor.
Preferably, in step c, inert atmosphere refers to argon gas or nitrogen.
Preferably, in step c, 1300 DEG C of reduction temperature, recovery time 50min.
Preferably, in order to realize recycling for reducing agent, save the cost, in step d, the reducing agent after screening returns to step
It is continued to use in rapid b.
Preferably, in step f, the organic solvent for cleaning the remaining reducing agent of the sub- titania surface of granular Magn é li phase can
To use ethyl alcohol.The selection of organic solvent mainly considers the cleaning effect to graphite, as long as other organic solvents can be effective
Cleaning graphite can be with.
The present invention also provides a kind of sub- titanium oxide of high-purity Magn é li phase, using the sub- titanium oxide of above-mentioned high-purity Magn é li phase
Preparation method be prepared.The sub- titanium oxide of high-purity Magn é li phase produced by the present invention, purity >=99%, the C content in product
≤ 0.46%.
Beneficial effects of the present invention:
1, the sub- titanium oxide of high-purity Magn é li phase is prepared in air atmosphere, is not needed vacuum or is passed through protective gas, it is right
Production equipment and production environment require low.
2, this technique can prepare the sub- titanium oxide of high-purity Magn é li phase in the shorter recovery time (30~60min).
3, method and process of the invention is simple, and cost of material is low and raw material reserves are huge, and the process is convenient for extensive
Industrial production.
4, the present invention prepares the sub- titanium oxide of high-purity Magn é li phase, and with high purity, residual carbon content is low.
Detailed description of the invention
Product XRD diagram prepared by Fig. 1 present example 1；
Product XRD diagram prepared by Fig. 2 present example 2；
Product XRD diagram prepared by Fig. 3 present example 3；
Specific embodiment
The technical problem to be solved in the present invention is to provide a kind of carbothermic method to prepare the sub- titanium oxide of high-purity Magn é li phase
Method.Core of the invention is to utilize the grain between graphite powder (reducing agent) and titanium dioxide granule using the method being granulated
It is poor to spend, and realizes and prepares the sub- titanium oxide of high-purity Magn é li phase using carbo-thermal process, to overcome traditional carbon thermal reduction product
Carbon residue is difficult to remove to obtain the technical problem of high purity product.
The preparation method of the sub- titanium oxide of high-purity Magn é li phase, sequentially includes the following steps:
A, by TiO2It mixes, pelletizes by weight 1:0.05~0.1 with binder, drying, obtaining diameter is 2~5mm
Grain A；
B, particle A and reducing agent are pressed into one layer of reducing agent, one layer of particle A, are staggeredly put into reactor, and top layer covers
Layer is reducing agent；Wherein, reducing agent is graphite powder or coal dust；A layers of particle are all made of monolayer of particles A covering, and cladding thickness is
The diameter of particle A；In addition to top layer's reducing agent, cladding thickness >=2cm of every layer of reducing agent；The cladding thickness of top layer's reducing agent
≥10cm；Granularity≤74 μm of reducing agent；
C, reactor is placed in 30~60min of reduction at 1250~1450 DEG C, reactor is taken out after reduction in inertia
It is cooling in atmosphere, obtain reduzate；
D, reduzate is sieved, obtains the sub- titanium oxide of granular Magn é li phase and reducing agent；
F, the remaining reducing agent of the sub- titania surface of granular Magn é li phase is cleaned, the sub- oxygen of high purity granular Magn é li phase is obtained
Change titanium.
The present invention needs first by TiO2The reason of granulation, granulation is that titanium dioxide and graphite powder (reducing agent) is made to generate granularity
Difference, to reduzate can be made to efficiently separate with the complete graphite powder of unreacted by the way of screening after reduction.Also,
The present invention needs the diameter by particle A to be limited within the scope of 2~5mm, and diameter is excessive too small to will affect sub- titanium oxide obtained
Purity.Particle A diameter is bigger, is unfavorable for inside CO gas transport to particle, does not fill to react within certain recovery time
Point, cause part TiO2It does not restore, to influence reduzate purity；When the diameter of particle A is too small (≤2mm), it will affect
The separation of product Magn é li phase sub- titanium oxide and graphite powder causes the sub- titanium oxide purity of the Magn é li phase of preparation not high.
The present invention is to expand graphite powder and TiO using the purpose of two kinds of layers of material interfoldeds2The contact of particle
Area improves reduction process dynamics, shortens the recovery time.
The granularity of granularity≤74 μm for the reducing agent that the present invention uses, reducing agent is smaller, and activity is higher when the condition of high temperature, has
Conducive to the formation and holding of entire reaction system reducing atmosphere, be conducive to the progress of reaction.And can make titanium dioxide with
It is poor that reducing agent generates granularity, to can make reduzate and the complete graphite powder of unreacted by the way of screening after reduction
It efficiently separates.
Preferably, in step a, binder is polyvinyl alcohol, and polyvinyl alcohol can be analyzed to H in the high temperature process2O and CO2,
The purity of product is not influenced.
In order to improve preparation sub- titanium oxide purity, it is preferred that TiO2With binder by weight 1:0.05.
In order to improve the degree that titanium dioxide is converted into sub- titanium oxide, the purity of sub- titanium oxide is improved, it is preferred that step a
In, the diameter of particle A is 2.5~5mm；It is furthermore preferred that the diameter of particle A is 2.5mm.
In order to improve the degree that titanium dioxide is converted into sub- titanium oxide, the purity of sub- titanium oxide is improved, it is preferred that step a
In, TiO2Purity is 99% or more.
In order to improve the degree that titanium dioxide is converted into sub- titanium oxide, the sub- titanium oxide of product Magn é li phase obtained is improved
Purity, it is preferred that in step b, every layer of reducing agent cladding thickness is 2.2~3cm, and the cladding thickness of top layer's reducing agent is
12~15cm；When every layer of reducing agent cladding thickness be 2.2cm, and the cladding thickness of top layer's reducing agent be 12cm, be made at this time
Product in C content it is minimum.
Preferably, in step b, reactor is graphiote reactor.
Preferably, in step c, inert atmosphere refers to argon gas or nitrogen.
In order to improve the degree that titanium dioxide is converted into sub- titanium oxide, the purity of sub- titanium oxide is improved, it is preferred that step c
In, 1300 DEG C of reduction temperature, recovery time 50min.
Preferably, in order to realize recycling for reducing agent, save the cost, in step d, the reducing agent after screening returns to step
It is continued to use in rapid b.
Preferably, in step f, the organic solvent for cleaning the remaining reducing agent of the sub- titania surface of granular Magn é li phase can
To use ethyl alcohol.The selection of organic solvent mainly considers the cleaning effect to graphite, as long as other organic solvents can be effective
Cleaning graphite can be with.
The present invention also provides a kind of sub- titanium oxide of high-purity Magn é li phase, using the sub- titanium oxide of above-mentioned high-purity Magn é li phase
Preparation method be prepared.The sub- titanium oxide of high-purity Magn é li phase produced by the present invention, purity >=99%, content of graphite≤
0.46%.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
In following embodiment, granularity≤74 μm of used graphite powder；Binder is polyvinyl alcohol.
Embodiment 1
Take 100gTiO2, 5g binder pelletizes after mixing and dries obtained particle A, and the diameter of particle A is 2.5mm；
Particle A and graphite powder are staggeredly placed in graphite crucible by one layer of graphite powder, one layer of particle A again, and top layer's coating is stone
Layer of toner；Wherein, in addition to top layer's graphite bisque, every layer of graphite powder cladding thickness is 2.2cm, and the covering of top layer's graphite bisque is thick
Degree is 12cm, and particle A coating is the particle A of single layer, and cladding thickness is the diameter 2.5mm of particle A；Then by graphite crucible
It is placed in high temperature furnace, in air atmosphere, 1300 DEG C of reduction temperature, recovery time 50min, after reaching the recovery time, by crucible
Argon gas protection is quickly removed and be passed through, is cooled to room temperature, reduzate is sieved, obtains the sub- oxidation of granular Magn é li phase
Titanium, then cleaning and fine grinding are carried out using dehydrated alcohol to the sub- titanium oxide of granular Magn é li phase, obtain the sub- oxygen of high-purity Magn é li phase
Change titanium products.The XRD diagram of product is shown in Fig. 1, it was demonstrated that its object phase composition is sub- titanium oxide.Product is tested, the present embodiment
The content of residual carbon is 0.17% in product.
Embodiment 2
Take 100gTiO2, 10g binder pelletizes after mixing and dries obtained particle A, and the diameter of particle A is 2mm,
Particle A and graphite powder are staggeredly placed in graphite crucible by one layer of graphite powder, one layer of particle A again, and top layer's coating is stone
Layer of toner；Wherein, in addition to top layer's graphite bisque, every layer of graphite powder cladding thickness is 2.5cm, and the covering of top layer's graphite bisque is thick
Degree is 12cm, and particle A coating is the particle A, cladding thickness 2mm of single layer；Then graphite crucible is placed in high temperature furnace,
Under air atmosphere, 1350 DEG C of reduction temperature, recovery time 40min after reaching the recovery time, crucible is quickly removed and is passed through argon
Gas shielded is cooled to room temperature, and is sieved to reduzate, the sub- titanium oxide of granular Magn é li phase is obtained, to granular Magn é
The sub- titanium oxide of li phase carries out cleaning and fine grinding using dehydrated alcohol, obtains the sub- titanium oxide product of high-purity Magn é li phase.Product
XRD diagram is shown in Fig. 2, it was demonstrated that its object phase composition is sub- titanium oxide.Product is tested, residual carbon contains in the product of the present embodiment
Amount is 0.46%.
Embodiment 3
Take 100gTiO2, 10g binder pelletizes after mixing and dries obtained particle A, and the diameter of particle A is 5mm,
Particle A and graphite powder are staggeredly placed in graphite crucible by one layer of graphite powder, one layer of particle A again, and top layer's coating is stone
Layer of toner；Wherein, in addition to top layer's graphite bisque, every layer of graphite powder cladding thickness is 3cm, top layer's graphite bisque cladding thickness
For 15cm, particle A coating is the particle A, cladding thickness 5mm of single layer；Then graphite crucible is placed in high temperature furnace, in sky
Under gas atmosphere, 1400 DEG C of reduction temperature, recovery time 30min after reaching the recovery time, crucible is quickly removed and is passed through argon gas
Protection, is cooled to room temperature, sieves to reduzate, the sub- titanium oxide of granular Magn é li phase is obtained, to granular Magn é li
Mutually sub- titanium oxide carries out cleaning and fine grinding using dehydrated alcohol, obtains the sub- titanium oxide product of high-purity Magn é li phase.The XRD of product
Figure is shown in Fig. 3, it was demonstrated that its object phase composition is sub- titanium oxide.Product is tested, the content of residual carbon in the product of the present embodiment
It is 0.27%.
Claims (10)
1. the preparation method of the sub- titanium oxide of high-purity Magn é li phase, which is characterized in that sequentially include the following steps:
A, by TiO2It mixes, pelletizes by weight 1:0.05~0.1 with binder, drying obtains the particle A that diameter is 2~5mm；
B, particle A and reducing agent are pressed into one layer of reducing agent, one layer of particle A, are staggeredly put into reactor, and top layer's coating is
Reducing agent；Wherein, reducing agent is graphite powder or coal dust；A layers of particle are all made of monolayer of particles A covering, and cladding thickness is particle A
Diameter；In addition to top layer's reducing agent, cladding thickness >=2cm of every layer of reducing agent；The cladding thickness of top layer's reducing agent >=
10cm；Granularity≤74 μm of reducing agent；
C, reactor is placed in 30~60min of reduction at 1250~1450 DEG C, reactor is taken out after reduction in inert atmosphere
Middle cooling, obtains reduzate；
D, reduzate is sieved, obtains the sub- titanium oxide of granular Magn é li phase and reducing agent；
F, the remaining reducing agent of the sub- titania surface of granular Magn é li phase is cleaned, the sub- titanium oxide of high-purity Magn é li phase is obtained.
2. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1, it is characterised in that: in step a,
Binder is polyvinyl alcohol.
3. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1 or 2, which is characterized in that step a
In: the diameter of particle A is 2.5~5mm；Preferably, the diameter of particle A is 2.5mm.
4. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1 or 2, which is characterized in that step a
In: TiO2Purity is 99% or more.
5. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to any one of claims 1 to 4, which is characterized in that
In step b, every layer of reducing agent cladding thickness is 2.2~3cm, and the cladding thickness of top layer's reducing agent is 12~15cm；It is preferred that
, every layer of reducing agent cladding thickness is 2.2cm, and the cladding thickness of top layer's reducing agent is 12cm.
6. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1 or 2, it is characterised in that: step b
In, reactor is graphiote reactor.
7. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1 or 2, it is characterised in that: step c
In, inert atmosphere refers to argon gas or nitrogen.
8. the preparation method of the sub- titanium oxide of described in any item high-purity Magn é li phases according to claim 1~7, it is characterised in that:
In step c, 1300 DEG C of reduction temperature, recovery time 50min.
9. the preparation method of the sub- titanium oxide of high-purity Magn é li phase according to claim 1, which is characterized in that in step d,
It is continued to use in reducing agent return step b after screening.
10. the sub- titanium oxide of high-purity Magn é li phase, which is characterized in that sub- using high-purity Magn é li phase described in claim 1~9
The preparation method of titanium oxide is prepared.
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Cited By (1)
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| CN111514875A (en) * | 2020-05-06 | 2020-08-11 | 青岛理工大学 | Three-dimensional electrode based on titanium tetroxide catalytic particles and application thereof in sewage treatment |
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