CN110629048A - Niobium tube production process - Google Patents
Niobium tube production process Download PDFInfo
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- CN110629048A CN110629048A CN201911065745.5A CN201911065745A CN110629048A CN 110629048 A CN110629048 A CN 110629048A CN 201911065745 A CN201911065745 A CN 201911065745A CN 110629048 A CN110629048 A CN 110629048A
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- Prior art keywords
- niobium
- solution
- tantalum
- pure
- organic phase
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/10—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies
- C21D8/105—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of tubular bodies of ferrous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/24—Obtaining niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a niobium tube production process, which takes niobium pentoxide and steel as raw materials, and is characterized by comprising three steps of pure niobium preparation, pure niobium purification and niobium tube production, and has the beneficial effects that: according to the invention, the purity of pure niobium is effectively improved by purifying the pure niobium, so that the waste of raw materials caused by the fact that the welding performance and hardness of the produced niobium tube cannot meet the requirements due to the low purity of the pure niobium in the traditional processing technology is avoided, and the reagent in the purification process can be repeatedly utilized, so that the cost in the niobium tube production technology is effectively saved, the manufacturing method can be widely popularized, and limited resources are saved.
Description
Technical Field
The invention discloses a niobium tube production process, and belongs to the technical field of niobium tube manufacturing processes.
Background
In the prior art, metal niobium can be prepared by electrolytic melting potassium heptafluoroniobate, or can be prepared by reducing potassium heptafluoroniobate by metal sodium or reducing niobium pentoxide by metal aluminum, and niobium is doped into steel, so that the oxidation resistance of the steel at high temperature can be improved, and the welding performance of the steel can be improved.
Disclosure of Invention
The invention aims to solve the technical problem and provides a niobium pipe production process, wherein the purity of pure niobium is effectively improved by purifying the pure niobium, so that the waste of raw materials caused by the fact that the welding performance and hardness of the produced niobium pipe cannot meet the requirements due to the fact that the purity of the pure niobium is not high in the traditional processing process is avoided, reagents in the purification process can be repeatedly utilized, the cost in the niobium pipe production process is effectively saved, the manufacturing method can be widely popularized, limited resources are saved, and the problems are solved.
In order to achieve the purpose, the invention provides the following technical scheme: a niobium tube production process takes niobium pentoxide and steel as raw materials and mainly comprises the following steps:
1) preparing pure niobium: mixing and stirring niobium pentoxide and aluminum powder, carrying out aluminothermic reaction between the niobium pentoxide and the aluminum powder at high temperature, filtering impurities to obtain pure niobium, and putting the obtained pure niobium liquid into an electron tube to remove residual gas in the pure niobium liquid.
2) And (3) purifying pure niobium:
A. performing partial secondary extraction on the pure niobium solution by using an organic mixed liquid phase consisting of 40% of N-503 and 60% of kerosene in a volume ratio, using 1.3-1.6moL/LH2SO4 and 2-3moL/LHF solution under a low-acid condition, SO that 30-40% of niobium-fluorine complex in the pure niobium solution and 80-90% of residual tantalum-fluorine complex are extracted into an organic phase to form a loaded organic phase mixed solution, and obtaining a low-tantalum-niobium solution with the tantalum content in the residual water phase remarkably reduced;
B. carrying out secondary niobium and tantalum extraction on niobium and a small amount of tantalum which enter an organic phase during partial secondary extraction in the process A, wherein the method comprises the steps of doping pure water into a loaded organic phase mixed solution, carrying out back extraction on niobium into a water phase again, carrying out back extraction on a trace amount of tantalum and niobium, and then extracting the trace amount of tantalum in the back-extracted niobium solution into the organic phase again by using a no-load N-503 organic phase to obtain a low-impurity niobium solution with high niobium back-extracted solution purity;
C. after the secondary niobium removal, washing the generated organic phase containing a small amount of tantalum-fluorine complex with 1-1.5% of NH4F solution to back extract tantalum into a water phase, returning the no-load organic phase to the initial stage of the A process, and performing new secondary extraction and tantalum extraction to obtain a pure niobium solution with high purity.
3) Manufacturing a niobium tube: and mixing and melting the pure niobium solution obtained in the step with a steel metal solution and other metal solutions, shaping by using a die, and annealing, cold rolling and cold drawing the shaped niobium pipe to obtain the required niobium pipe.
Preferably, the niobium pentoxide is obtained from mined ores by separation, so that the niobium pentoxide and tantalum pentoxide are separated from other minerals.
Preferably, the temperature of the thermite reaction between the niobium pentoxide and the aluminum powder is 800-1000 ℃.
Preferably, the mixing ratio of the pure niobium solution to the steel metal solution and the other metal solutions is 0.03:0.96: 0.01.
Preferably, the particle diameter of the aluminum powder is 5-20 um.
Compared with the prior art, the invention has the following beneficial effects:
the method effectively improves the purity of the pure niobium by purifying the pure niobium, thereby avoiding the waste of raw materials caused by the fact that the welding performance and the hardness of a produced niobium pipe can not meet the requirements due to the low purity of the pure niobium in the traditional processing technology, wherein an organic mixed liquid phase consisting of 40 percent N-503 and 60 percent kerosene by volume ratio is adopted in the purification of the pure niobium, 1.3-1.6moL/LH2SO4 and 2-3moL/LHF solution are used for carrying out partial secondary extraction on the pure niobium liquid under the low-acid condition, SO that 30-40 percent of niobium-fluorine complex in the pure niobium liquid and 80-90 percent of residual tantalum-fluorine complex are extracted into an organic phase to form a loaded organic phase mixed liquid, SO as to obtain a low-niobium tantalum liquid with the tantalum content obviously reduced in the water phase, and the purification of the pure niobium is carried out by secondary niobium reverse reaction and repeated utilization of the tantalum, thereby greatly improving the purity of the niobium, the cost in the niobium tube production process is effectively saved, so that the manufacturing method can be widely popularized, and limited resources are saved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A niobium tube production process takes niobium pentoxide and steel as raw materials and mainly comprises the following steps:
1) preparing pure niobium: mixing and stirring niobium pentoxide and aluminum powder, carrying out aluminothermic reaction between the niobium pentoxide and the aluminum powder at high temperature, filtering impurities to obtain pure niobium, and putting the obtained pure niobium liquid into an electron tube to remove residual gas in the pure niobium liquid.
2) And (3) purifying pure niobium:
A. performing partial secondary extraction on the pure niobium solution by using an organic mixed liquid phase consisting of 40% of N-503 and 60% of kerosene in a volume ratio, using 1.3-1.6moL/LH2SO4 and 2-3moL/LHF solution under a low-acid condition, SO that 30-40% of niobium-fluorine complex in the pure niobium solution and 80-90% of residual tantalum-fluorine complex are extracted into an organic phase to form a loaded organic phase mixed solution, and obtaining a low-tantalum-niobium solution with the tantalum content in the residual water phase remarkably reduced;
B. carrying out secondary niobium and tantalum extraction on niobium and a small amount of tantalum which enter an organic phase during partial secondary extraction in the process A, wherein the method comprises the steps of doping pure water into a loaded organic phase mixed solution, carrying out back extraction on niobium into a water phase again, carrying out back extraction on a trace amount of tantalum and niobium, and then extracting the trace amount of tantalum in the back-extracted niobium solution into the organic phase again by using a no-load N-503 organic phase to obtain a low-impurity niobium solution with high niobium back-extracted solution purity;
C. after the secondary niobium removal, washing the generated organic phase containing a small amount of tantalum-fluorine complex with 1-1.5% of NH4F solution to back extract tantalum into a water phase, returning the no-load organic phase to the initial stage of the A process, and performing new secondary extraction and tantalum extraction to obtain a pure niobium solution with high purity.
3) Manufacturing a niobium tube: and mixing and melting the pure niobium solution obtained in the step with a steel metal solution and other metal solutions, shaping by using a die, and annealing, cold rolling and cold drawing the shaped niobium pipe to obtain the required niobium pipe.
Wherein the niobium pentoxide is obtained from mined ores after separation, so that the niobium pentoxide and tantalum pentoxide are separated from other minerals.
Wherein the temperature of the thermite reaction of the niobium pentoxide and the aluminum powder is 800-1000 ℃.
Wherein the mixing ratio of the pure niobium solution to the steel metal solution and the other metal solutions is 0.03:0.96: 0.01.
Wherein the particle diameter of the aluminum powder is 5-20 um.
Specifically, when the niobium pentoxide and the aluminum powder are mixed and stirred in the use process, an aluminothermic reaction is carried out between the niobium pentoxide and the aluminum powder under the condition of high temperature, the impurities in the niobium pentoxide and the aluminum powder are filtered to obtain pure niobium, the obtained pure niobium liquid is put into an electronic tube to remove residual gas, an organic mixed liquid phase consisting of 40% of N-503 and 60% of kerosene in volume ratio is used, 1.3-1.6moL/LH2SO4 and 2-3moL/LHF solution are used for carrying out partial secondary extraction under the condition of low acid, 30-40% of niobium-fluorine complex in the pure niobium liquid and 80-90% of residual tantalum-fluorine complex are extracted into an organic phase to form a loaded organic phase mixed solution, a low-tantalum-niobium liquid with the tantalum content remarkably reduced in a water phase is obtained, and the niobium and a small amount of tantalum which enter the organic phase during partial secondary extraction in the process A are subjected to secondary niobium-reverse extraction, The method for extracting tantalum comprises the steps of firstly doping pure water into the mixed liquid of the loaded organic phase, back-extracting niobium into the water phase, simultaneously back-extracting trace tantalum and niobium, then re-extracting the trace tantalum in the niobium back-extraction solution into an organic phase by using an unloaded N-503 organic phase to obtain a low-impurity niobium solution with high niobium back-extraction solution purity, and after secondary niobium back-extraction, washing the generated organic phase containing a small amount of tantalum-fluorine complex with 1-1.5% NH4F solution to back extract tantalum into the water phase, returning the no-load organic phase to the initial stage of the process A for new secondary extraction and tantalum extraction, thereby obtaining pure niobium solution with high purity, mixing and melting the pure niobium solution obtained in the step with steel metal solution and other metal solution, and (3) shaping by using a die, and annealing, cold rolling and cold drawing the shaped niobium pipe to obtain the required niobium pipe.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A niobium tube production process takes niobium pentoxide and steel as raw materials and is characterized in that: the method mainly comprises the following steps:
1) preparing pure niobium: mixing and stirring niobium pentoxide and aluminum powder, carrying out aluminothermic reaction between the niobium pentoxide and the aluminum powder at a high temperature, filtering impurities to obtain pure niobium, and putting the obtained pure niobium liquid into an electron tube to remove residual gas in the pure niobium liquid;
2) and (3) purifying pure niobium: A. performing partial secondary extraction on the pure niobium solution by using an organic mixed liquid phase consisting of 40% of N-503 and 60% of kerosene in a volume ratio, using 1.3-1.6moL/LH2SO4 and 2-3moL/LHF solution under a low-acid condition, SO that 30-40% of niobium-fluorine complex in the pure niobium solution and 80-90% of residual tantalum-fluorine complex are extracted into an organic phase to form a loaded organic phase mixed solution, and obtaining a low-tantalum-niobium solution with the tantalum content in the residual water phase remarkably reduced;
B. carrying out secondary niobium and tantalum extraction on niobium and a small amount of tantalum which enter an organic phase during partial secondary extraction in the process A, wherein the method comprises the steps of doping pure water into a loaded organic phase mixed solution, carrying out back extraction on niobium into a water phase again, carrying out back extraction on a trace amount of tantalum and niobium, and then extracting the trace amount of tantalum in the back-extracted niobium solution into the organic phase again by using a no-load N-503 organic phase to obtain a low-impurity niobium solution with high niobium back-extracted solution purity;
C. after the secondary niobium removal, washing the generated organic phase containing a small amount of tantalum-fluorine complex with 1-1.5% of NH4F solution to back extract tantalum into a water phase, returning the no-load organic phase to the initial stage of the A process, and performing new secondary extraction and tantalum extraction to obtain a pure niobium solution with high purity.
3) Manufacturing a niobium tube: and mixing and melting the pure niobium solution obtained in the step with a steel metal solution and other metal solutions, shaping by using a die, and annealing, cold rolling and cold drawing the shaped niobium pipe to obtain the required niobium pipe.
2. The niobium pipe production process as claimed in claim 1, wherein: the niobium pentoxide is obtained from mined ores by separation, so that the niobium pentoxide and tantalum pentoxide are separated from other minerals.
3. The niobium pipe production process as claimed in claim 1, wherein: the temperature of the thermite reaction of the niobium pentoxide and the aluminum powder is 800-1000 ℃.
4. The niobium pipe production process as claimed in claim 1, wherein: the mixing ratio of the pure niobium solution to the steel metal solution and the other metal solutions is 0.03:0.96: 0.01.
5. The niobium pipe production process as claimed in claim 1, wherein: the particle diameter of the aluminum powder is 5-20 um.
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| CN201911065745.5A CN110629048A (en) | 2019-11-04 | 2019-11-04 | Niobium tube production process |
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| CN201911065745.5A CN110629048A (en) | 2019-11-04 | 2019-11-04 | Niobium tube production process |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076731A (en) * | 1992-03-06 | 1993-09-29 | H.C施塔克公司 | The method of isolating tantalum and niobium |
| CN1594611A (en) * | 2004-06-24 | 2005-03-16 | 株洲硬质合金集团有限公司 | Niobium purifying method |
| CN101215635A (en) * | 2007-01-05 | 2008-07-09 | 中国科学院过程工程研究所 | Method for separating tantalum and niobium from potassium metatantalate and potassium metaniobate mixture |
| CN102399990A (en) * | 2011-11-28 | 2012-04-04 | 镇江中孚复合材料有限公司 | Method for extracting niobium oxide from waste and old niobium-containing high-temperature alloy |
| CN103898386A (en) * | 2014-03-31 | 2014-07-02 | 承德天大钒业有限责任公司 | Aluminum-molybdenum-niobium-copper-zirconium intermediate alloy and preparation method thereof |
| CN105385866A (en) * | 2015-12-15 | 2016-03-09 | 赣州有色冶金研究所 | Preparation method and system of niobium-aluminium alloy |
-
2019
- 2019-11-04 CN CN201911065745.5A patent/CN110629048A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076731A (en) * | 1992-03-06 | 1993-09-29 | H.C施塔克公司 | The method of isolating tantalum and niobium |
| CN1594611A (en) * | 2004-06-24 | 2005-03-16 | 株洲硬质合金集团有限公司 | Niobium purifying method |
| CN100489125C (en) * | 2004-06-24 | 2009-05-20 | 株洲硬质合金集团有限公司 | Niobium purifying method |
| CN101215635A (en) * | 2007-01-05 | 2008-07-09 | 中国科学院过程工程研究所 | Method for separating tantalum and niobium from potassium metatantalate and potassium metaniobate mixture |
| CN102399990A (en) * | 2011-11-28 | 2012-04-04 | 镇江中孚复合材料有限公司 | Method for extracting niobium oxide from waste and old niobium-containing high-temperature alloy |
| CN103898386A (en) * | 2014-03-31 | 2014-07-02 | 承德天大钒业有限责任公司 | Aluminum-molybdenum-niobium-copper-zirconium intermediate alloy and preparation method thereof |
| CN105385866A (en) * | 2015-12-15 | 2016-03-09 | 赣州有色冶金研究所 | Preparation method and system of niobium-aluminium alloy |
Non-Patent Citations (1)
| Title |
|---|
| 泽里克曼: "《稀散金属冶金学》", 30 September 1982 * |
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