CN105130432A - Production method of body material crucible for calcining hydroxides in tantalum and niobium smelting - Google Patents
Production method of body material crucible for calcining hydroxides in tantalum and niobium smelting Download PDFInfo
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- CN105130432A CN105130432A CN201510443238.6A CN201510443238A CN105130432A CN 105130432 A CN105130432 A CN 105130432A CN 201510443238 A CN201510443238 A CN 201510443238A CN 105130432 A CN105130432 A CN 105130432A
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- die
- crucible
- calcining
- punch
- production method
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- 238000001354 calcination Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title abstract description 13
- 238000003723 Smelting Methods 0.000 title abstract 2
- 150000004679 hydroxides Chemical class 0.000 title abstract 2
- 229910052758 niobium Inorganic materials 0.000 title abstract 2
- 239000010955 niobium Substances 0.000 title abstract 2
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title abstract 2
- 229910052715 tantalum Inorganic materials 0.000 title abstract 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title abstract 2
- 238000004806 packaging method and process Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000004033 plastic Substances 0.000 claims abstract description 5
- 229920003023 plastic Polymers 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 16
- 230000035939 shock Effects 0.000 claims description 13
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 claims description 11
- 239000007858 starting material Substances 0.000 claims description 10
- 239000013590 bulk material Substances 0.000 claims description 8
- RHDUVDHGVHBHCL-UHFFFAOYSA-N niobium tantalum Chemical compound [Nb].[Ta] RHDUVDHGVHBHCL-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 241001062472 Stokellia anisodon Species 0.000 claims description 6
- 238000003837 high-temperature calcination Methods 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 6
- 239000002985 plastic film Substances 0.000 claims description 6
- 229920006255 plastic film Polymers 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 150000003951 lactams Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 238000000462 isostatic pressing Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Press-Shaping Or Shaping Using Conveyers (AREA)
Abstract
The invention discloses a production method of a body material crucible for calcining hydroxides in tantalum and niobium smelting. The production method includes the steps of material blending, primary moulding, primary hydraulic treatment, vacuumizing packaging with plastic membrane, primary isostatic pressing treatment, microwave drying, and high-temperature roasting. The production method is stable in moulding. A crucible product is uniform in shape and wall thickness and is excellent in compactness. The production method is convenient and quick, is simple in operations, saves labor intensity and manual work, is less in investment cost, is short in production period, allows batched production and can reduce labor cost.
Description
Technical field
The present invention relates to the calcining of a kind of tantalum niobium hydrometallurgy, especially a kind of tantalum-niobium smelt calcining oxyhydroxide bulk material crucible making method.
Background technology
The metallurgical the finished product oxide compound of tantalum niobium is obtained through calcining by oxyhydroxide, and the product foreign matter content after calcining requires to only have several PPM.Realizing continuous calcining adopts the crucible splendid attire oxyhydroxide made by bulk material oxide compound to produce usually.It is by taking bulk material oxide compound as starting material through batching, Pulp preparation, the operation such as shaping that the crucible used at present makes.Wherein this making link shaping is the key link that crucible makes, due to oxide flow difference so be difficult to shaping.Mostly the making method of current crucible is to adopt traditional ceramic preparation method, and its shaping size and wall thickness are difficult to control, and the production cycle is long, production efficiency is low, and yield rate is low.The present invention is directed to above manufacture craft to improve production efficiency and quality, shorten the production cycle.
Summary of the invention
A kind of tantalum-niobium smelt is the object of the present invention is to provide to calcine oxyhydroxide bulk material crucible making method.
Technical scheme of the present invention is: a kind of tantalum-niobium smelt calcining oxyhydroxide bulk material crucible making method, its step: batching, pre-profiling, hydraulic pressure, plastic film vacuumize packaging, isostatic pressed, microwave drying, high-temperature calcination.
(1) prepare burden:
Starting material niobium hydroxide is used hydraulic efficiency installation briquetting in a mold, and pressure is 0.25MPa;
1) block oxyhydroxide is sintered into oxide compound, calcining temperature is 600 ° ~ about 800 °;
2) broken after calcining normal temperature of coming out of the stove, then sieve with 450 eye mesh screens: select+450 ~-60 order particles; Be unscreened the further fragmentation of the material fallen to sieve and select+450 ~-60 orders;
3) starting material after sieving add polyvinyl lactam: 3% ~ 5%, water: 6% ~ 8% stirs batch mixing.
(2) pre-profiling: complete crucible germule by vibrations rotating mold and make
1) rotating mold comprises pedestal, vertical vibrating motor, shock platforms, swing bearing, die, punch; Be provided with shock platforms above pedestal, be provided with vertical vibrating motor in the middle of pedestal, vibration motor is crossed gusset plate and is connected with pedestal, and pedestal is connected with shock platforms by spring; Shock platforms is provided with swing bearing, and die, punch are connected with shock platforms by punch support; Pedestal shakes spring with gusset plate bottom vibrations frame by 12 and connects, and vertical vibrating motor is connected with vibrations frame by 8 bolts with gusset plate bottom vibrations frame.Swing bearing is fixed in the shock platforms of vibrations frame by the bolt-connection of 8 on inner ring revolving support.Backing plate is connected and fixed by 8 bolts and swing bearing cycle hole.Crucible die is connected and fixed by 5 bolts and backing plate 4.Punch is fixed on punch support by 5 bolt-connections, and punch support is arranged in shock platforms by 3 bolts; Push pedal is by bolt) and spring and die be connected to form the ejecting mechanism of product;
2) working method: starter motor, in the even blanking in die end face groove place, drives die at the uniform velocity to rotate by swing bearing simultaneously, when material is charged to die groove position, fills material and terminates.
(3) once extrude: (utilizing the quick once shaped of oil press)
Previous step equipment is pulled down punch support and punch, taking-up die, the die that germule is housed is arranged on and installs on the hydropress of punch, start hydraulic efficiency installation, complete once shaped.
(4) plastic film vacuumizes packaging
Operating process: after a shaped by fluid pressure, releases stock with the ejecting mechanism push pedal of die; Stock is loaded in plastics bag to vacuumize and pack; For next step isostatic pressed is prepared, prevent highly pressurised liquid oil immersion to stock.
(5) post forming: (isostatic pressed)
Operating process: put into isostatic pressed high pressure vessel after packaged product is put into A-frame; Starting equal pressing equipment pressure is 300MPa, 3 minutes dwell times.
(6) microwave drying:
Take packaging after isostatic pressed apart product is put into microwave oven to dry.Bake out temperature: 80 ° ~ 100 °, the time: 60 ~ 90 minutes.
(7) high-temperature calcination:
Product after oven dry is put into pusher furnace calcine, calcining temperature is respectively: niobium oxides crucible: 1150 °; Tantalum oxide crucible: 1450 ° ~ 1480 °; Calcination time: 1 ~ 2 hour.
The invention has the advantages that: stable molding, shape of product and uniform wall thickness, crucible compactness are good, convenient and swift, simple to operate, human-saving, less manpower, investment are little, with short production cycle, can be mass, reduce labour cost.
Accompanying drawing explanation
Fig. 1 is that the present invention shakes rotating mold structural representation;
Fig. 2 is oil press of the present invention and mould sketch.
Embodiment
A kind of tantalum-niobium smelt calcining oxyhydroxide bulk material crucible making method, its step: batching, pre-profiling, hydraulic pressure, plastic film vacuumize packaging, isostatic pressed, microwave drying, high-temperature calcination.
(1) prepare burden:
1) starting material niobium hydroxide is used hydraulic efficiency installation briquetting in a mold, pressure is 0.25MPa;
2) block oxyhydroxide is sintered into oxide compound, calcining temperature is 600 ° ~ about 800 °;
3) broken after calcining normal temperature of coming out of the stove, then sieve with 450 eye mesh screens: select+450 ~-60 order particles; Be unscreened the further fragmentation of the material fallen to sieve and select+450 ~-60 orders;
Starting material after sieving add polyvinyl lactam: 3% ~ 5%, water: 6% ~ 8% stirs batch mixing; Above step solves mobility, the plastic problems of oxide compound.
(2) pre-profiling: complete crucible germule by vibrations rotating mold and make
1) rotating mold comprises pedestal, vertical vibrating motor, shock platforms, swing bearing, die, punch; Pedestal 15 shakes spring 14 with gusset plate 12 bottom vibrations frame by 12 and connects, vertical vibrating motor 13 is connected with vibrations frame by 8 bolts with gusset plate 12 bottom vibrations frame 11, swing bearing is fixed in the shock platforms 8 of vibrations frame 11 by the bolt-connection of 8 on inner ring revolving support 7, backing plate 4 is connected and fixed by 8 bolts and hole, swing bearing outer ring 6, crucible die 2 is connected and fixed by 5 bolts and backing plate 4, punch 1 is fixed on punch support 3 by 5 bolt-connections, and punch support 3 is arranged in shock platforms by 3 bolts; Push pedal 5 is connected to form the ejecting mechanism of product by bolt 10 and spring 9 with die;
2) working method: starter motor, in the even blanking in die end face groove place, drives die at the uniform velocity to rotate by swing bearing simultaneously, when material is charged to die groove position, fills material and terminates;
(3) once extrude:
Previous step equipment is pulled down punch support 3 and punch 16, takes out die 2, the die 2 that germule is housed is arranged on the hydropress installing punch 16, start hydraulic efficiency installation, complete once shaped;
(4) plastic film vacuumizes packaging
Operating process: after a shaped by fluid pressure, releases stock with the ejecting mechanism push pedal of die; Stock is loaded in plastics bag to vacuumize and pack; For next step isostatic pressed is prepared, prevent highly pressurised liquid oil immersion to stock.
(5) post forming: (isostatic pressed)
Operating process: put into isostatic pressed high pressure vessel after packaged product is put into A-frame; Starting equal pressing equipment pressure is 300MPa, 3 minutes dwell times.
(6) microwave drying
Take packaging after isostatic pressed apart product is put into microwave oven to dry.Bake out temperature: 80 ° ~ 100 °, the time: 60 ~ 90 minutes.Object: remove moisture in product.
(7) high-temperature calcination
Product after oven dry is put into pusher furnace calcine.Calcining temperature is respectively: niobium oxides crucible: 1150 °; Tantalum oxide crucible: 1450 ° ~ 1480 °; Calcination time: 1 ~ 2 hour.
(8) precaution:
1) need control during pre-profiling that swing bearing rotating speed is even and blanking velocity is even.
2) after die cavity fills material, fill margin can be increased at die groove place, avoid after punching press the defects such as stock Density inhomogeneity.
3) note the secondary location of die during hydraulic pressure, avoid dynamic and static mould eccentric.
4) to control the release dynamics of push rod and speed during the demoulding well, avoid demoulding failure or damage blank.
Claims (1)
1. a tantalum-niobium smelt calcining oxyhydroxide bulk material crucible making method, its step: batching, pre-profiling, hydraulic pressure, plastic film vacuumize packaging, isostatic pressed, microwave drying, high-temperature calcination;
(1) prepare burden:
Starting material niobium hydroxide is used hydraulic efficiency installation briquetting in a mold, and pressure is 0.25MPa;
1) block oxyhydroxide is sintered into oxide compound, calcining temperature is 600 ° ~ about 800 °;
2) broken after calcining normal temperature of coming out of the stove, then sieve with 450 eye mesh screens: select+450 ~-60 order particles; Be unscreened the further fragmentation of the material fallen to sieve and select+450 ~-60 orders;
3) starting material after sieving add polyvinyl lactam: 3% ~ 5%, water: 6% ~ 8% stirs batch mixing;
(2) pre-profiling: complete crucible germule by vibrations rotating mold and make:
1) rotating mold comprises pedestal, vertical vibrating motor, shock platforms, swing bearing, die, punch, pedestal (15) shakes spring (14) with gusset plate (12) bottom vibrations frame by 12 and connects, vertical vibrating motor (13) is connected with vibrations frame by 8 bolts with vibrations frame (11) bottom gusset plate (12), swing bearing is fixed in the shock platforms (8) of vibrations frame (11) by 8 bolt-connections on inner ring revolving support (7), backing plate (4) is connected and fixed by 8 bolts and swing bearing outer ring (6) hole, crucible die (2) is connected and fixed by 5 bolts and backing plate (4), punch (1) is fixed on punch support (3) by 5 bolt-connections, punch support (3) is arranged in shock platforms by 3 bolts, push pedal (5) is connected to form the ejecting mechanism of product by bolt (10) and spring (9) with die,
2) working method: starter motor, in the even blanking in die end face groove place, drives die at the uniform velocity to rotate by swing bearing simultaneously, when material is charged to die groove position, fills material and terminates;
(3) once extrude:
Previous step equipment is pulled down punch support (3) and punch (16), takes out die (2), the die (2) that germule is housed is arranged on the hydropress installing punch (16), start hydraulic efficiency installation, complete once shaped;
(4) plastic film vacuumizes packaging:
Operating process: after a shaped by fluid pressure, releases stock with the ejecting mechanism push pedal of die; Stock is loaded in plastics bag to vacuumize and pack; For next step isostatic pressed is prepared, prevent highly pressurised liquid oil immersion to stock;
(5) post forming:
Operating process: put into isostatic pressed high pressure vessel after packaged product is put into A-frame; Starting equal pressing equipment pressure is 300MPa, 3 minutes dwell times;
(6) microwave drying:
Take packaging after isostatic pressed apart product is put into microwave oven to dry, bake out temperature: 80 ° ~ 100 °, time: 60 ~ 90 minutes;
(7) high-temperature calcination:
Product after oven dry is put into pusher furnace calcine, calcining temperature is respectively: niobium oxides crucible: 1150 °; Tantalum oxide crucible: 1450 ° ~ 1480 °; Calcination time: 1 ~ 2 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510443238.6A CN105130432B (en) | 2015-07-27 | 2015-07-27 | A kind of tantalum-niobium smelt calcines hydroxide bulk material crucible preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510443238.6A CN105130432B (en) | 2015-07-27 | 2015-07-27 | A kind of tantalum-niobium smelt calcines hydroxide bulk material crucible preparation method |
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| Publication Number | Publication Date |
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| CN105130432A true CN105130432A (en) | 2015-12-09 |
| CN105130432B CN105130432B (en) | 2017-06-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358631A (en) * | 2018-02-02 | 2018-08-03 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity tantalum oxide ontology crucible |
| CN108530066A (en) * | 2018-04-10 | 2018-09-14 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity niobium oxide ontology crucible |
| CN109292822A (en) * | 2018-12-17 | 2019-02-01 | 株洲硬质合金集团有限公司 | A kind of preparation method of High-density Niobium Oxide |
-
2015
- 2015-07-27 CN CN201510443238.6A patent/CN105130432B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358631A (en) * | 2018-02-02 | 2018-08-03 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity tantalum oxide ontology crucible |
| CN108530066A (en) * | 2018-04-10 | 2018-09-14 | 九江有色金属冶炼有限公司 | A kind of manufacturing method of high purity niobium oxide ontology crucible |
| CN109292822A (en) * | 2018-12-17 | 2019-02-01 | 株洲硬质合金集团有限公司 | A kind of preparation method of High-density Niobium Oxide |
| CN109292822B (en) * | 2018-12-17 | 2021-01-26 | 株洲硬质合金集团有限公司 | Preparation method of niobium pentoxide with high apparent density |
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| Publication number | Publication date |
|---|---|
| CN105130432B (en) | 2017-06-30 |
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Effective date of registration: 20180906 Address after: 336000 No. 3 Chun Yi Road, Yichun economic and Technological Development Zone, Jiangxi Patentee after: Jiangxi Tuo Hong new materials Co., Ltd. Address before: 338000 Dongxing North Road, Xinyu hi tech Development Zone, Jiangxi Patentee before: JIANGXI SANSHI NONFERROUS METALS CO., LTD. |