CN102380619A - Method for reducing impurity content in tantalum powder produced by sodium reducing method - Google Patents
Method for reducing impurity content in tantalum powder produced by sodium reducing method Download PDFInfo
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- CN102380619A CN102380619A CN2011103057879A CN201110305787A CN102380619A CN 102380619 A CN102380619 A CN 102380619A CN 2011103057879 A CN2011103057879 A CN 2011103057879A CN 201110305787 A CN201110305787 A CN 201110305787A CN 102380619 A CN102380619 A CN 102380619A
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- tantalum powder
- koh
- molten salt
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Abstract
The invention discloses a method for reducing impurity content in tantalum powder produced by a sodium reducing method. In the method, KOH is added into a molten salt system, wherein 5-25g of KOH is added to every 100kg of dilute salt. In the invention, KOH is added into every 100kg of dilute salt and enters the molten salt system; and a little amount of HF2- reaction exists between the KOH and the molten salt system, and the hydrolysis of KF is inhibited so as to reduce corrosion of a reaction tank caused by the molten salt system and reduce the content of impurities including iron, nickel and chromium in the tantalum powder.
Description
Technical field:
The invention belongs to the metal smelt field, be specifically related to a kind of method that reduces impurity content in the tantalum powder that sodium reduction produces.
Background technology:
Capacitor tantalum powder is one of primary raw material of making by electrolytic capacitor.Because it is high that liquid-liquid stirring potassium floutaramite sodium reduction is produced the tantalum powder specific volume that the method production capacity of tantalum powder is big, controllability good, produce, therefore, manufacturer generally adopts this method production capacitor tantalum powder both at home and abroad at present.But this method has an outstanding shortcoming, and iron in the tantalum powder of promptly producing in the ordinary course of things, nickel, chromium impurity content are higher, if do not remove, will influence the final electrical property quality of product.
Contain iron, nickel, chromium impurity in the tantalum powder; Its reason is in the molten salt system of potassium floutaramite reduction, to be dissolved with iron, nickel, chromium ion; And the main source of these ions, the one, raw material and diluent are carried secretly, and the 2nd, the reduction apparatus surface is corroded and makes and is dissolved with these ions in the fused salt.If guarantee raw material and diluent higher purity is arranged, then the source of iron, nickel, chromium impurity is that reduction apparatus is corroded in the tantalum powder.The oxide of potassium floutaramite and wherein free hydrogen fluoric acid, sodium metal and sodium, the high temperature corrosion effect of peroxide; Stir the wearing and tearing of stirring arm in the reduction; Mechanical entrainments in operating process such as material stripping, fragmentation etc. all make iron, nickel, chromium metal in the structural material get in the tantalum powder.Except get into stainless steel or the bits of other materials in the tantalum powder because of mechanical wear, be outside existing with metallic state, most of iron, nickel, chromium have a then more complicated of form, possibly be that the compound state exists, also possibly form alloy or intermetallic compound with tantalum.
In order to reduce impurity content in the tantalum powder, each tantalum powder manufacturer has at first given great attention to the resistance to corrosion of equipment, and the anti-corrosion material of high-quality is used in the production process of tantalum powder.Raw material K
2TaF
7New technology has also been developed in the production that reaches diluent, has used new material, makes its impurity content also obtain reducing significantly.Simultaneously both at home and abroad all Application and Development in reduction process, avoid the technology of corrosion reaction equipment, significantly reduced the Fe in the sodium reduction tantalum powder, Ni, Cr, C content.
Summary of the invention:
The purpose of this invention is to provide a kind of method that reduces impurity content in the tantalum powder that sodium reduction produces.
The method of impurity content is characterized in that in the tantalum powder that reduction sodium reduction of the present invention is produced, and may further comprise the steps:
In molten salt system, add KOH, the adding method is in every 100kg diluting salt, to add the form of 5～25g KOH.
Preferably, in every 100kg diluting salt, add 10g KOH.
The present invention is through adding KOH in every 100kg diluting salt, KOH gets into molten salt system, the small amount of H F that exists in KOH and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort, reduce the content of iron, nickel, chromium impurity in the tantalum powder.
Know-why of the present invention is: add KOH in the diluting salt, following reaction: 2KF+H takes place in it
2O=2K
++ OH
-+ HF
2 -HF
2 -At high temperature be decomposed into HF
-, reaction equation is HF
2 -=H
++ 2F
-H under the high temperature
+Retort is produced certain corrosion, following reaction: 2K takes place behind the adding KOH
++ OH
-+ HF
2 -=2KF+H
2O; OH
-When excessive, thereby the hydrolysis that can suppress KF reduces HF
2 -Growing amount, reduce H
+Growing amount, make H
+The corrosion that retort is produced reduces, and reduces the content of iron, nickel, chromium impurity in the tantalum powder.
After in every 100kg diluting salt, adding the KOH of different amounts, and then stir the potassium floutaramite sodium reduction according to liquid-liquid of routine and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is as shown in table 1:
Table 1:KOH amount is to the influence of tantalum powder impurity content
| Add KOH amount (g) | 0 | 5 | 10 | 15 | 20 | 25 | 40 |
| Fe, Ni, Cr impurity content (ppm) | 50 | 32 | 18 | 26 | 40 | 42.5 | 60 |
Can find out that by table 1 after adding a certain amount of KOH in every 100kg diluting salt, the content of the iron in the tantalum powder, nickel, chromium impurity can reduce, and, can produce new corrosion retort when surpassing a certain amount of the time.The amount that therefore need in every 100kg diluting salt, add 5～25g KOH is the most suitable, and optimum is that every 100kg diluting salt adds 10g KOH.
The present invention adds a certain amount of KOH in molten salt system after, effectively reduced the content of iron in the tantalum powder, nickel, chromium impurity, prepared high-quality tantalum powder condition is provided for utilizing liquid-liquid to stir the potassium floutaramite sodium reduction.
The specific embodiment:
Below be to further specify to of the present invention, rather than limitation of the present invention.
Comparative Examples 1:
In molten salt system, do not add KOH, stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Comparative Examples 2:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 40g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Embodiment 1:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 5g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Embodiment 2:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 10g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Embodiment 3:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 15g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Embodiment 4:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 20g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Embodiment 5:
In molten salt system, add KOH, the adding method is to join in the molten salt system with the form that in every 100kg diluting salt, adds 25g KOH, makes the small amount of H F that exists in itself and the molten salt system
2 -Reaction, and the hydrolysis of inhibition KF, thus the corrosion of molten salt system reduced to retort; And then stir the potassium floutaramite sodium reduction according to the liquid of routine-liquid and prepare the tantalum powder, the content of the iron in the tantalum powder, nickel, chromium impurity is seen table 1.
Claims (2)
1. a method that reduces impurity content in the tantalum powder that sodium reduction produces is characterized in that may further comprise the steps: in molten salt system, add KOH, the adding method is in every 100kg diluting salt, to add the form of 5～25g KOH.
2. the method for impurity content is characterized in that in the tantalum powder that reduction sodium reduction according to claim 1 is produced, and in every 100kg diluting salt, adds 10g KOH.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103057879A CN102380619A (en) | 2011-10-10 | 2011-10-10 | Method for reducing impurity content in tantalum powder produced by sodium reducing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103057879A CN102380619A (en) | 2011-10-10 | 2011-10-10 | Method for reducing impurity content in tantalum powder produced by sodium reducing method |
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|---|---|
| CN102380619A true CN102380619A (en) | 2012-03-21 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4149876A (en) * | 1978-06-06 | 1979-04-17 | Fansteel Inc. | Process for producing tantalum and columbium powder |
| US4684399A (en) * | 1986-03-04 | 1987-08-04 | Cabot Corporation | Tantalum powder process |
| JP2004156060A (en) * | 2002-11-01 | 2004-06-03 | Cabot Supermetal Kk | Method for producing metal powder, and method for evaluating raw material or diluted salt used therefor |
| CN101879603A (en) * | 2010-06-18 | 2010-11-10 | 江门富祥电子材料有限公司 | Production method and production device of tantalum powder |
-
2011
- 2011-10-10 CN CN2011103057879A patent/CN102380619A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4149876A (en) * | 1978-06-06 | 1979-04-17 | Fansteel Inc. | Process for producing tantalum and columbium powder |
| US4684399A (en) * | 1986-03-04 | 1987-08-04 | Cabot Corporation | Tantalum powder process |
| JP2004156060A (en) * | 2002-11-01 | 2004-06-03 | Cabot Supermetal Kk | Method for producing metal powder, and method for evaluating raw material or diluted salt used therefor |
| CN1720114A (en) * | 2002-11-01 | 2006-01-11 | 卡伯特超金属株式会社 | Method for preparing metal powder and method for evaluating raw material or diluting salt for use therein |
| CN101879603A (en) * | 2010-06-18 | 2010-11-10 | 江门富祥电子材料有限公司 | Production method and production device of tantalum powder |
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Application publication date: 20120321 |
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