CN107416885B - A kind of method of electric smelting method production cerium oxide - Google Patents

A kind of method of electric smelting method production cerium oxide Download PDF

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Publication number
CN107416885B
CN107416885B CN201710315501.2A CN201710315501A CN107416885B CN 107416885 B CN107416885 B CN 107416885B CN 201710315501 A CN201710315501 A CN 201710315501A CN 107416885 B CN107416885 B CN 107416885B
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cerium oxide
electric smelting
raw material
electric
melting
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CN107416885A (en
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胡天喜
叶旦旺
包晓刚
程诗忠
李小毅
初薛基
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SANXIANG ADVANCED MATERIALS CO Ltd
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SANXIANG ADVANCED MATERIALS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/90Other properties not specified above

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The present invention relates to a kind of methods of electric smelting method production cerium oxide, cerium oxide raw material is put into batches and carries out melting in electric arc furnaces, controlling electrode voltage when melting is 110-270V, electric current 2-15kA, puts into next group raw material again after last consignment of raw material all fusing, after the completion of melting, heat preservation 0-2 hours, current control when heat preservation is in 200-500A, and then furnace cooling obtains frit, by frit by being crushed, except iron cleans and grinds, the electric smelting cerium oxide of varigrained sand shape or powdery is obtained.Present invention process process is simple, production cost is low, other impurities will not be introduced in production process or generate pernicious gas, very well satisfy enterprise to low cost, high efficiency, environmental protection production requirement, and the purity of obtained electric smelting cerium oxide is up to 98% or more, the product porosity is less than 2%, and bulk density is up to 7.5g/cm3More than, compressive resistance is up to 80MPa or more.

Description

A kind of method of electric smelting method production cerium oxide
Technical field
The present invention relates to the preparation field of special refractories, specifically a kind of method of electric smelting method production cerium oxide.
Background technique
The oxide of cerium mainly has a ceria and two kinds of cerium sesquioxide, ceria can be aoxidized by cerium sesquioxide and At, be relatively stable cerium oxide, therefore, commonly referred to as cerium oxide when refer mainly to ceria, the oxidation mentioned in the present invention Cerium or electric smelting cerium oxide, refer to ceria.
Common ceria oxide powder because under stomata height and high temperature shrink etc. factors be difficult to use at high temperature, limit its The application of fire resisting material field.It can be usually prepared at present by sintering process as the cerium oxide that refractory material uses, compared to general Lead to ceria oxide powder, the porosity of cerium oxide made from sintering process is lower, and generally 5% or so, bulk density is higher, generally 7.21g/cm3, the high temperature resistance and thermal stability of product can basically meet the requirement of conventional refractory materials.But it burns Sintering time needed for connection is longer, and process flow is complex, and impurity is readily incorporated in sintering process and is easy to produce pollution Gas, thus be unable to satisfy enterprise to low cost, high efficiency, environmental protection production requirement, and the purity of product is than common oxygen It is low to change cerium, the porosity and consistency also have to be hoisted, limit it in the application in higher level such as special refractories field, nothing Method meets the requirement of the special refractories in the fields such as aerospace, military project, scientific research, optics, electronics.
Summary of the invention
In order to overcome the defects of the prior art described above, technical problem to be solved by the invention is to provide it is a kind of low cost, High efficiency, environmental protection electric smelting method production cerium oxide method, cerium oxide made from this method has that purity is high, the porosity be low, body The features such as product density is big, high temperature resistant, thermal stability and mechanical property are good, the use that can meet special refractories well is wanted It asks.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows:
A kind of method of electric smelting method production cerium oxide, cerium oxide raw material is put into batches and carries out melting in electric arc furnaces, is controlled Electrode voltage when melting is 110-270V, electric current 2-15kA, puts into next group original again after last consignment of raw material all fusing Material after the completion of melting, keeps the temperature 0-2 hour, and current control when heat preservation is in 200-500A, and then furnace cooling obtains frit, general Frit is cleaned and is ground by being crushed, removing iron, obtains the electric smelting cerium oxide of varigrained sand shape or powdery.
The beneficial effects of the present invention are: it is different from the prior art, the present invention can be by common oxidation using electric smelting method Cerium powder is prepared into electric smelting cerium oxide, and process flow is simple, and production cost is low, and other impurities or production will not be introduced in production process Raw pernicious gas, very well satisfy enterprise to low cost, high efficiency, environmental protection production requirement, and obtained electric smelting oxygen Change the purity of cerium up to 98% or more, the product porosity is less than 2%, and bulk density is up to 7.5g/cm3More than, compressive resistance can Up to 80MPa or more, has the characteristics that big purity is high, bulk density, high temperature resistant, thermal stability and mechanical property are good, can be applied to The special refractories in the fields such as aerospace, military project, scientific research, optics, electronics, can also preparation structure ceramics and function ceramics.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The most critical design of the present invention is: preparing cerium oxide using electric smelting method, and rationally design smelting technology and heat preservation Technique enables electric smelting cerium oxide to prepare, and electric smelting cerium oxide obtained is with high purity, bulk density is big, resistance to height Temperature, the features such as thermal stability and mechanical property are good.
Specifically, the method for electric smelting method production cerium oxide provided by the invention, puts into electric arc furnaces for cerium oxide raw material in batches Middle carry out melting, controlling electrode voltage when melting is 110-270V, electric current 2-15kA, after last consignment of raw material all fusing Next group raw material is put into again, after the completion of melting, keeps the temperature 0-2 hours, and current control when heat preservation is then cold with furnace in 200-500A But frit is obtained, by frit by being crushed, except iron cleans and grinds, obtains the electric smelting oxidation of varigrained sand shape or powdery Cerium.
By test, using the purity of electric smelting cerium oxide obtained by above-mentioned electric smelting method up to 98% or more, product stomata Rate is less than 2%, and bulk density is up to 7.5g/cm3, compressive resistance far superior to common ceria oxide powder and adopts up to 80MPa The cerium oxide made from sintering process, made special refractories can obtain good in the smelting and casting of titanium alloy Effect, titanium part mass ratio is more excellent using conventional refractory materials, and can be widely applied to aerospace, military project, scientific research, optics, electricity The special refractories in the fields such as son, it can also be used to preparation structure ceramics and function ceramics.
As can be seen from the above description, the beneficial effects of the present invention are: it is different from the prior art, the present invention can using electric smelting method Common ceria oxide powder is prepared into electric smelting cerium oxide, process flow is simple, and production cost is low, will not draw in production process Enter other impurities or generate pernicious gas, very well satisfy enterprise to low cost, high efficiency, environmental protection production requirement, and The purity of obtained electric smelting cerium oxide is up to 98% or more, and the product porosity is less than 2%, and bulk density is up to 7.5g/cm3With On, compressive resistance has purity is high, bulk density are big, high temperature resistant, thermal stability and mechanical property are good etc. up to 80MPa or more Feature can be applied to the special refractories in the fields such as aerospace, military project, scientific research, optics, electronics, can also preparation structure pottery Porcelain and function ceramics.
Further, the purity of the cerium oxide raw material is greater than 98wt%.
As can be seen from the above description, the beneficial effects of the present invention are: it is greater than the cerium oxide raw material of 98wt% using purity, it can To ensure that the electric smelting cerium oxide of high-purity is made.Compared to existing sintering process, since the present invention will not introduce in process of production Other impurities, therefore electric smelting cerium oxide obtained can keep well the purity of raw material, and meet special refractories Requirement.
Further, in fusion process, by adjusting the power of electrode, in-furnace temperature is made to be maintained at 2300 DEG C -2400 ℃。
As can be seen from the above description, the beneficial effects of the present invention are: by controlling in-furnace temperature at 2300 DEG C -2400 DEG C, the quality of product can be made more stable.
Further, in insulating process, inert gas is passed through into furnace to replace gas original in loss of sheet, and make furnace Interior air pressure is increased to 0.5~1MPa.
As can be seen from the above description, the beneficial effects of the present invention are: gas original in loss of sheet is replaced using inert gas, Introduced contaminants can effectively be completely cut off, and inert gas will not be reacted with cerium oxide, further improve the purity of product.Separately Outside, at a high pressure condition, the crystalline arrangement of cerium oxide is closer, advantageously reduces the porosity of product, improves the body of product Product density.
Further, the inert gas is nitrogen, helium or argon gas.
Embodiment 1
Raw material cerium oxide (purity 99.99%) is put into electric arc furnaces in batches and carries out melting, coordination electrode voltage is 110V, electric current 2kA, at 2300 DEG C or more, the raw material being added at first starts to melt smelting temperature, continues to feed, continues to melt Change, until raw material is all added and melted, melt liquid carries out heat preservation 1 hour (heat preservation current control 200A), then certainly with furnace So cooling obtains frit.Frit is finally obtained into varigrained sand or powder by being crushed, except iron cleans and grinds.
After tested, electric smelting cerium oxide made from the embodiment 1,99.8% or more, the product porosity is less than finished product purity 2%, bulk density is up to 7.5g/cm3, compressive resistance is up to 80MPa.
Embodiment 2
Raw material cerium oxide (purity 98.5%) is put into electric arc furnaces in batches and carries out melting, coordination electrode voltage is 110V, electric current 2kA, at 2300 DEG C or more, the raw material being added at first starts to melt smelting temperature, continues to feed, continues to melt Change, until raw material is all added and melted, then obtains frit with furnace natural cooling.Finally by frit by being crushed, except iron removes Miscellaneous and grinding, obtains varigrained sand or powder.
After tested, electric smelting cerium oxide made from the embodiment 2,98.3% or more, the product porosity is less than finished product purity 2%, bulk density is up to 7.3g/cm3, compressive resistance is up to 55MPa.
Embodiment 3
Raw material cerium oxide (purity 99%) is put into electric arc furnaces in batches and carries out melting, coordination electrode voltage is 110V, Electric current is 2kA, and at 2300 DEG C or more, the raw material being added at first starts to melt smelting temperature, continues to feed, continues to melt, and is melted The power that electrode is adjusted during refining, makes in-furnace temperature remain at 2300 DEG C -2400 DEG C, until raw material is all added and melted Change, then keep voltage constant, by current reduction to 200-500A, keep the temperature 2 hours, heat preservation while be passed through into furnace nitrogen, Helium or argon gas make air pressure in furnace be increased to 0.5~1MPa to replace gas original in loss of sheet, then with furnace natural cooling Obtain frit.Frit is finally obtained into varigrained sand or powder by being crushed, except iron cleans and grinds.
After tested, electric smelting cerium oxide made from the embodiment 3,98.9% or more, the product porosity does not surpass finished product purity 1.5% is crossed, bulk density is up to 7.7g/cm3More than, compressive resistance is up to 90MPa or more.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair In bright scope of patent protection.

Claims (4)

1. a kind of method of electric smelting method production cerium oxide, it is characterised in that: put into electric arc furnaces cerium oxide raw material in batches and carry out Melting, controlling electrode voltage when melting is 110-270V, electric current 2-15kA, is put into again after last consignment of raw material all fusing Next group raw material after the completion of melting, keeps the temperature 0-2 hours, and current control when heat preservation is in 200-500A, and then furnace cooling obtains Frit obtains the electric smelting cerium oxide of varigrained sand shape or powdery by frit by being crushed, except iron cleans and grinds;Molten During refining, by adjusting the power of electrode, in-furnace temperature is made to be maintained at 2300 DEG C -2400 DEG C.
2. the method for electric smelting method according to claim 1 production cerium oxide, it is characterised in that: the cerium oxide raw material it is pure Degree is greater than 98wt%.
3. the method for electric smelting method production cerium oxide according to claim 1, it is characterised in that: in insulating process, to furnace It is passed through inert gas inside to replace gas original in loss of sheet, and air pressure in furnace is made to be increased to 0.5~1MPa.
4. the method for electric smelting method production cerium oxide according to claim 3, it is characterised in that: the inert gas is nitrogen Gas, helium or argon gas.
CN201710315501.2A 2017-05-08 2017-05-08 A kind of method of electric smelting method production cerium oxide Active CN107416885B (en)

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CN101857261A (en) * 2010-06-29 2010-10-13 上海大学 Method for preparing nano Ce(OH)3 powder
CN102275972A (en) * 2011-06-07 2011-12-14 上海大学 Preparation method of Mn-doped CeO2 nano powder
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