CN106929697A - A kind of purifying technique of pure niobium - Google Patents
A kind of purifying technique of pure niobium Download PDFInfo
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- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
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- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
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Abstract
The invention discloses a kind of purifying technique of pure niobium, using microcomputer online monitoring system, equipment is set to be greatly improved the guaranteed extent of technique；Impurity content is further reduced in making niobium oxide, using thermite reaction institute liberated heat, dystectic niobium melting is deposited to reactor bottom, and is purified again by electronic torch melting, to obtain the melting niobium of higher degree；In addition, can effectively remove low-melting-point metal impurity by refining；The large crystal grain niobium ingot that will be obtained after electronic torch melting is cut directly into big crystal grain niobium sheet, then niobium sheet surface is chemically treated；That eliminate conventional fabrication processes process and the techniques such as the cogging of large crystal grain niobium ingot elder generation, annealing are made the steps such as little crystal grain niobium plate and electrochemical polish, avoid processing pollution, and its RRR value of obtained niobium sheet is suitable with ingot casting, improves superconductivity, accelerating gradient and performance higher is obtained.
Description
Technical field
The present invention relates to a kind of purifying technique of pure niobium, belong to niobium purification technique field.
Background technology
Niobium belongs to rare precious metal, with its fusing point is high, corrosion resistance is good, good processing characteristics, thermal-neutron capture cross-section
The features such as small, good heat conductivity, high emitting performance and pumping property, it is widely used in steel, electronics industry, aviation, low
The field such as temperature superconductive and nuclear industry；In recent years, information industry and microelectric technique developing rapidly and high level steel product needed
The sustainable growth asked, for the development of hydrometallurgy provides fabulous opportunity；But simultaneously there is serious fluoride pollution in current technology
And the low problem of resolution ratio of low-grade tantalum niobium concentrate, increasingly govern the development of hydrometallurgy；And in the purification process of niobium
In, there is the problems such as reaction condition is undesirable, and processing step is not rigorous, cause the purification purity of niobium not to be too high, containing more
Impurity, and cost for purification is also higher, inefficiency, does not meet actual production requirement.Therefore, in order to solve problem above,
Urgently propose that a kind of pollution is small, and yield pure niobium high purification process.
The content of the invention
To solve the above problems, the present invention proposes a kind of purifying technique of pure niobium, is released using thermite reaction
Heat, the melting of dystectic niobium is deposited to reactor bottom, and purified again by electronic torch melting, to obtain higher degree
Melting niobium；Low-melting-point metal impurity can effectively be removed by refining, the superconductivity of niobium is improve, acceleration higher is obtained
Gradient and performance.
The purifying technique of pure niobium of the invention, the process is comprised the following steps：
Step one, niobium is smelted,
The first step, hydrometallurgy,
A. Feedstock treating, chooses tantalum-niobium concentrate, and concentrate is ground by vibrator, obtains tantalum niobium concentrate powder；
B. acid is decomposed, and HF-H is measured using bailing bucket flowmeter2SO4Solution, and tantalum niobium concentrate powder is placed in HF-H2SO4In solution
Decomposed, obtained decomposed solution；
C. extract, after decomposed solution is through acid adjustment, extracted in novel combination type extractor using organic solvent, tantalum, niobium
Into organic phase, and the major part impurities left such as iron, silicon, tungsten, titanium, manganese is in water phase slurry；
D. pickling, takes the organic phase after extraction, and impurity is removed through overpickling, is stripped with anti-niobium liquid and obtains fluooxycolumbic acid water
Solution, then organic phase containing tantalum is stripped with anti-tantalum liquid, the fluorotantalic acid aqueous solution is obtained, and analyze molten across limit analyzer using X-ray
Whether there is tantalum in liquid；
E. pickling again is strengthened, to adding HF-H again in the solution after pickling2SO4Solution, the pickling operation to previous step enters
Row reinforcing, further goes the removal of impurity；
F. precipitate, fluorotantalic acid solution is heated up, acid adjustment, and continuous spray precipitation is carried out with ammonia produce the low fluorine tantalum niobium of bulky grain
Oxide, chemical equation is as follows：
2H2[NbOF5]+10NH4OH→Nb2O5↓+10NH4F+7H2O；
G. pyrohydrolytic method's fluorine removal, to the water vapour that purification is passed through in material, makes the fluoride generation fluorination of remaining in material
Hydrogen and ammonia and discharge so that fluorine is reduced to less than 0.001% in material；
H. filter, wash, the low fluorine tantalum niobium oxide of bulky grain after precipitation is placed in filter plant, and inhaled by biology
Attaching organism membrane filter method is filtered, and is washed using ionized water after filtering,
I. dry, the low fluorine tantalum niobium oxide of bulky grain after filtration washing is put into drying plant to be carried out at heating, drying
Reason；
J. it is calcined, the tantalum niobium oxide after drying is obtained Nb by calcining2O5；
K. cool down, using steel body rotational moulding groove to the Nb after roasting2O5Force to cool down by chilled water, obtain Nb2O5Crystallization；
Second step, thermit reduction production metal niobium,
A. batch mixing, the Nb that will be obtained in the first step2O5Mix with aluminium powder, obtain batch mixing；
B. reduction reaction, takes the batch mixing of previous step, and the alloy of niobium and aluminium is obtained by reduction reaction, and is entered by disintegrating machine
Row break process, reduction reaction equation is as follows：
3Nb2O5+ 10Al=6Nb+5Al2O3；
C. melting, use level electron beam furnace carries out melting treatment to broken rear material, is slightly melted niobium and its conjunction
Gold；
Step 2, Refining, using vacuum electron beam stove and arc-melting furnace under high temperature and high vacuum condition to step
Thick melting niobium and its alloy in rapid one using thermit reduction production are smelted, and obtain the niobium and its alloy pig of high-purity,
Low-melting-point metal impurity can be effectively removed, alloy intermediate gap impurity element (O, N, C, H etc.) content is reduced；
Step 3, processing, the niobium and its alloy pig of electronic torch melting and arc melting are first passed through according to the size of ingot blank
Large crystal grain niobium ingot is obtained after crossing preprocessing operation, then large crystal grain niobium ingot is placed on ingot casting the niobium material for cutting single crystal grain, used
The method for rolling, makes its diameter slowly expand, and is made a diameter of 266~270mm, and thickness is the niobium sheet of 3~3.5mm；Again to niobium
Piece surface makes its thickness reach 2.8~3mm by eliminating stress treatment, surface Vehicle Processing treatment and chemical treating process, obtains
High-purity niobium sheet.
Further, the concrete operation step of the pickling is to be less than 8N by the organic phase containing tantalum and niobium and containing acidity
H2SO4Fresh water mutually mixed；With this understanding, during only niobium is mutually stripped in water, and tantalum remains in organic phase；Instead
The hydration niobium of extraction reuses organic solvent extraction, to remove residual tantalum.
Further, the organic solvent is methyl iso-butyl ketone (MIBK), tributyl phosphate, cyclohexanone or sec-octyl alcohol.
Used as preferred embodiment, the organic solvent is methyl iso-butyl ketone (MIBK).
As preferred embodiment, microcomputer online monitoring system is provided with the filter plant and drying plant,
Equipment is set to be greatly improved the guaranteed extent of technique；Impurity content is further reduced in making niobium oxide, especially Gao Rong
The content of point metal impurities (Ta, W, Mo), for the control of Niobium Superconducting material refractory metal impurity content provides strong guarantee.
Used as preferred embodiment, the filter plant includes full automatic pressure filter and Gore membrane filtration machine.
Used as preferred embodiment, the drying plant includes coated infrared drier, rotatory vacuum dryer and hot blast
Circulation baking oven.
Used as preferred embodiment, the preprocessing operation is the various combination for forging, extrude, rolling or swaging.
Used as preferred embodiment, described its maximum gauge of large crystal grain niobium ingot is 120mm.
Compared with prior art, the purifying technique of pure niobium of the invention, using microcomputer online monitoring system, makes the present invention
Equipment is greatly improved to the guaranteed extent of technique；Impurity content is further reduced in making niobium oxide；Using aluminothermic reduction
Reaction institute liberated heat, makes dystectic niobium melting be deposited to reactor bottom, and is purified again by electronic torch melting, with
To the melting niobium of higher degree；In addition, can effectively remove low-melting-point metal impurity by refining；By what is obtained after electronic torch melting
Large crystal grain niobium ingot is cut directly into big crystal grain niobium sheet, then niobium sheet surface is chemically treated；That eliminate conventional fabrication processes
The cogging of large crystal grain niobium ingot elder generation, the technique such as annealing is made the steps such as little crystal grain niobium plate and electrochemical polish by process, it is to avoid process
Pollution, and its RRR value of obtained niobium sheet is suitable with ingot casting, improves the superconductivity of niobium, obtain accelerating gradient higher and
Performance.
Specific embodiment
Embodiment 1：
The purifying technique of pure niobium of the invention, the process is comprised the following steps：
Step one, niobium is smelted,
The first step, hydrometallurgy,
A. Feedstock treating, chooses tantalum-niobium concentrate, and concentrate is ground by vibrator, obtains tantalum niobium concentrate powder；
B. acid is decomposed, and HF-H is measured using bailing bucket flowmeter2SO4Solution, and tantalum niobium concentrate powder is placed in HF-H2SO4In solution
Decomposed, obtained decomposed solution；
C. extract, after decomposed solution is through acid adjustment, extracted in novel combination type extractor using organic solvent, tantalum, niobium
Into organic phase, and the major part impurities left such as iron, silicon, tungsten, titanium, manganese is in water phase slurry；
D. pickling, takes the organic phase after extraction, and impurity is removed through overpickling, is stripped with anti-niobium liquid and obtains fluooxycolumbic acid water
Solution, then organic phase containing tantalum is stripped with anti-tantalum liquid, the fluorotantalic acid aqueous solution is obtained, and analyze molten across limit analyzer using X-ray
Whether there is tantalum in liquid；
E. pickling again is strengthened, to adding HF-H again in the solution after pickling2SO4Solution, the pickling operation to previous step enters
Row reinforcing, further goes the removal of impurity；
F. precipitate, fluorotantalic acid solution is heated up, acid adjustment, and continuous spray precipitation is carried out with ammonia produce the low fluorine tantalum niobium of bulky grain
Oxide, chemical equation is as follows：
2H2[NbOF5]+10NH4OH→Nb2O5↓+10NH4F+7H2O；
G. pyrohydrolytic method's fluorine removal, to the water vapour that purification is passed through in material, makes the fluoride generation fluorination of remaining in material
Hydrogen and ammonia and discharge so that fluorine is reduced to less than 0.001% in material；
H. filter, wash, the low fluorine tantalum niobium oxide of bulky grain after precipitation is placed in filter plant, and inhaled by biology
Attaching organism membrane filter method is filtered, and is washed using ionized water after filtering,
I. dry, the low fluorine tantalum niobium oxide of bulky grain after filtration washing is put into drying plant to be carried out at heating, drying
Reason；
J. it is calcined, the tantalum niobium oxide after drying is obtained Nb by calcining2O5；
K. cool down, using steel body rotational moulding groove to the Nb after roasting2O5Force to cool down by chilled water, obtain Nb2O5Crystallization；
Second step, thermit reduction production metal niobium,
A. batch mixing, the Nb that will be obtained in the first step2O5Mix with aluminium powder, obtain batch mixing；
B. reduction reaction, takes the batch mixing of previous step, and the alloy of niobium and aluminium is obtained by reduction reaction, and is entered by disintegrating machine
Row break process, reduction reaction equation is as follows：
3Nb2O5+ 10Al=6Nb+5Al2O3；
C. melting, use level electron beam furnace carries out melting treatment to broken rear material, is slightly melted niobium and its conjunction
Gold；
Step 2, Refining, using vacuum electron beam stove and arc-melting furnace under high temperature and high vacuum condition to step
Thick melting niobium and its alloy in rapid one using thermit reduction production are smelted, and obtain the niobium and its alloy pig of high-purity；
Step 3, processing, the niobium and its alloy pig of electronic torch melting and arc melting are first passed through according to the size of ingot blank
Large crystal grain niobium ingot is obtained after crossing preprocessing operation, then large crystal grain niobium ingot is placed on ingot casting the niobium material for cutting single crystal grain, used
The method for rolling, makes its diameter slowly expand, and is made a diameter of 266mm, and thickness is the niobium sheet of 3~3.5mm；Again to niobium sheet surface
By eliminating stress treatment, surface Vehicle Processing treatment and chemical treating process, its thickness is reached 2.8mm, obtain high-purity
Niobium sheet.
The concrete operation step of the pickling is by the organic phase containing tantalum and niobium and the H containing acidity less than 8N2SO4It is new
Fresh water is mutually mixed；With this understanding, during only niobium is mutually stripped in water, and tantalum remains in organic phase；The water of back extraction
Close niobium and reuse organic solvent extraction, to remove residual tantalum.
Wherein, the organic solvent is methyl iso-butyl ketone (MIBK).Microcomputer is provided with the filter plant and drying plant
Online monitoring system.The filter plant includes full automatic pressure filter and Gore membrane filtration machine.The drying plant includes remote red
Outer dryer, rotatory vacuum dryer and heated-air circulation oven.The preprocessing operation is forged, extrudes, rolls or is swaged
Various combination.Described its maximum gauge of large crystal grain niobium ingot is 120mm.
The purifying technique of pure niobium of the invention, using microcomputer online monitoring system, makes equipment have the guaranteed extent of technique
Very big raising；Impurity content is further reduced in making niobium oxide, and especially refractory metal impurity (Ta, W, Mo) contains
Amount, for the control of Niobium Superconducting material refractory metal impurity content provides strong guarantee；Aluminothermic reduction has obvious heat release
Feature, thermite reaction reacts once igniting, and autoreactivity liberated heat can meet that reaction is spontaneous to be carried out, whole reaction
Process time is short, yield is big；Using reduction reaction institute liberated heat, dystectic niobium melting is set to be deposited to reactor bottom,
This thick niobium contains the metal impurities such as Fe, Ni, Al higher and O, N gas content, therefore is purified again by electronic torch melting, with
Obtain the melting niobium of higher degree；And not existing impurity C element in whole course of reaction, the melting niobium is for producing superconduction
With the optimum feed stock of High-purity Niobium ingot (RRR ＞ 300)；Low-melting-point metal impurity can effectively be removed by refining, reduced in the middle of alloy
Gap impurity element (O, N, C, H etc.) content；The large crystal grain niobium ingot that will be obtained after electronic torch melting is cut directly into big crystal grain niobium sheet,
Diameter 266mm is made, thickness is the piece of 2.8~3mm, then niobium sheet surface is chemically treated；That eliminate conventionally manufactured work
The cogging of large crystal grain niobium ingot elder generation, the technique such as annealing is made the steps such as little crystal grain niobium plate and electrochemical polish by skill process, it is to avoid add
Work pollutes, and its RRR value of obtained niobium sheet is suitable with ingot casting, improves superconductivity, obtains accelerating gradient and property higher
Energy.
Above-described embodiment, is only better embodiment of the invention, therefore all structures according to described in present patent application scope
Make, the equivalent change or modification that feature and principle are done, be included in the range of present patent application.
Claims (9)
1. a kind of purifying technique of pure niobium, it is characterised in that：The process is comprised the following steps：
Step one, niobium is smelted,
The first step, hydrometallurgy,
A. Feedstock treating, chooses tantalum-niobium concentrate, and concentrate is ground by vibrator, obtains tantalum niobium concentrate powder；
B. acid is decomposed, and HF-H is measured using bailing bucket flowmeter2SO4Solution, and tantalum niobium concentrate powder is placed in HF-H2SO4Carried out in solution
Decompose, obtain decomposed solution；
C. extract, after decomposed solution is through acid adjustment, extracted in novel combination type extractor using organic solvent, tantalum, niobium enter
Organic phase, and the major part impurities left such as iron, silicon, tungsten, titanium, manganese is in water phase slurry；
D. pickling, takes the organic phase after extraction, and impurity is removed through overpickling, and it is water-soluble to obtain fluooxycolumbic acid with the back extraction of anti-niobium liquid
Liquid, then organic phase containing tantalum is stripped with anti-tantalum liquid, the fluorotantalic acid aqueous solution is obtained, and judgement is analyzed across limit analyzer using X-ray
Whether there is tantalum in solution；
E. pickling again is strengthened, to adding HF-H again in the solution after pickling2SO4Solution, the pickling operation to previous step is carried out by force
Change, further go the removal of impurity；
F. precipitate, fluorotantalic acid solution is heated up, acid adjustment, and continuous spray precipitation is carried out with ammonia and produce the oxidation of bulky grain low fluorine tantalum niobium
Thing, chemical equation is as follows：
2H2[NbOF5]+10NH4OH→Nb2O5↓+10NH4F+7H2O；
G. pyrohydrolytic method's fluorine removal, to the water vapour that purification is passed through in material, makes the fluoride generation fluorination hydrogen of remaining in material
Body and ammonia and discharge so that fluorine is reduced to less than 0.001% in material；
H. filter, wash, the low fluorine tantalum niobium oxide of bulky grain after precipitation is placed in filter plant, and given birth to by biological adsorption
Thing membrane filter method is filtered, and is washed using ionized water after filtering,
I. dry, the low fluorine tantalum niobium oxide of bulky grain after filtration washing is put into drying plant carries out heating, drying treatment；
J. it is calcined, the tantalum niobium oxide after drying is obtained Nb by calcining2O5；
K. cool down, using steel body rotational moulding groove to the Nb after roasting2O5Force to cool down by chilled water, obtain Nb2O5Crystallization；
Second step, thermit reduction production metal niobium,
A. batch mixing, the Nb that will be obtained in the first step2O5Mix with aluminium powder, obtain batch mixing；
B. reduction reaction, takes the batch mixing of previous step, and the alloy of niobium and aluminium is obtained by reduction reaction, and is broken by disintegrating machine
Broken treatment, reduction reaction equation is as follows：
3Nb2O5+ 10Al=6Nb+5Al2O3；
C. melting, use level electron beam furnace carries out melting treatment to broken rear material, is slightly melted niobium and its alloy；
Step 2, Refining, using vacuum electron beam stove and arc-melting furnace under high temperature and high vacuum condition to step one
The thick melting niobium and its alloy of middle use thermit reduction production are smelted, and obtain the niobium and its alloy pig of high-purity；
Step 3, processing, the niobium and its alloy pig of electronic torch melting and arc melting is first passed through according to the size of ingot blank pre-
Large crystal grain niobium ingot is obtained after manufacturing procedure, then large crystal grain niobium ingot is placed on ingot casting the niobium material for cutting single crystal grain, using rolling
Method, its diameter is slowly expanded, be made a diameter of 266~270mm, thickness is the niobium sheet of 3~3.5mm；Again to niobium sheet table
Face makes its thickness reach 2.8~3mm by eliminating stress treatment, surface Vehicle Processing treatment and chemical treating process, obtains high-purity
Degree niobium sheet.
2. the purifying technique of pure niobium according to claim 1, it is characterised in that：The concrete operation step of the pickling be by
Organic phase containing tantalum and niobium and the H containing acidity less than 8N2SO4Fresh water mutually mixed；With this understanding, only niobium exists
During water is mutually stripped, and tantalum remains in organic phase；The hydration niobium of back extraction reuses organic solvent extraction, to remove residual
Tantalum.
3. the purifying technique of pure niobium according to claim 1, it is characterised in that：The organic solvent is methyl-isobutyl
Ketone, tributyl phosphate, cyclohexanone or sec-octyl alcohol.
4. the purifying technique of pure niobium according to claim 3, it is characterised in that：The organic solvent is methyl-isobutyl
Ketone.
5. the purifying technique of pure niobium according to claim 1, it is characterised in that：On the filter plant and drying plant
It is provided with microcomputer online monitoring system.
6. the purifying technique of pure niobium according to claim 1, it is characterised in that：The filter plant includes full-automatic press filtration
Machine and Gore membrane filtration machine.
7. the purifying technique of pure niobium according to claim 1, it is characterised in that：The drying plant includes far infrared drying
Machine, rotatory vacuum dryer and heated-air circulation oven.
8. the purifying technique of pure niobium according to claim 1, it is characterised in that：The preprocessing operation for forging, extruding,
The various combination for rolling or swaging.
9. the purifying technique of pure niobium according to claim 1, it is characterised in that：Described its maximum gauge of large crystal grain niobium ingot is
120mm。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107619955A (en) * | 2017-09-22 | 2018-01-23 | 宝鸡市博信金属材料有限公司 | The high-purity tantalum foil preparation methods of OLED |
| CN108046323A (en) * | 2017-12-20 | 2018-05-18 | 广东省稀有金属研究所 | A kind of preparation method of niobium oxide |
| CN110819827A (en) * | 2019-11-18 | 2020-02-21 | 常熟市振兴铸件有限公司 | Preparation process of niobium strip |
| CN113267043A (en) * | 2021-05-31 | 2021-08-17 | 稀美资源(广东)有限公司 | Drying and roasting integrated energy-saving production method |
| CN115466841A (en) * | 2022-04-13 | 2022-12-13 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity niobium sheet for irradiation supervision neutron detection |
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| CN107619955A (en) * | 2017-09-22 | 2018-01-23 | 宝鸡市博信金属材料有限公司 | The high-purity tantalum foil preparation methods of OLED |
| CN107619955B (en) * | 2017-09-22 | 2019-08-27 | 宝鸡市博信金属材料有限公司 | The high-purity tantalum foil preparation method of OLED |
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| CN108046323B (en) * | 2017-12-20 | 2019-08-02 | 广东省稀有金属研究所 | A kind of preparation method of niobium oxide |
| CN110819827A (en) * | 2019-11-18 | 2020-02-21 | 常熟市振兴铸件有限公司 | Preparation process of niobium strip |
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| CN115466841A (en) * | 2022-04-13 | 2022-12-13 | 宁夏东方钽业股份有限公司 | Preparation method of high-purity niobium sheet for irradiation supervision neutron detection |
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