CN101994131A - Method for producing metallic titanium - Google Patents
Method for producing metallic titanium Download PDFInfo
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- CN101994131A CN101994131A CN2009100130714A CN200910013071A CN101994131A CN 101994131 A CN101994131 A CN 101994131A CN 2009100130714 A CN2009100130714 A CN 2009100130714A CN 200910013071 A CN200910013071 A CN 200910013071A CN 101994131 A CN101994131 A CN 101994131A
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- metallic titanium
- titanium
- electrolysis
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- sponge
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Abstract
The invention provides a method for producing metallic titanium, particularly a method for preparing sponge metallic titanium through directly electrolyzing and reducing TiO2 by using a SOM (Solid Oxygen-permeation Membrane). The method for producing the sponge metallic titanium solves the problems of carbon pollution, low current efficiency and strict requirement on raw materials in an FFC (Flexible Flat Cable) method. The method adopted by the invention comprises the steps of exerting 3.2V voltage in an MgF2-CaF2 system of 1150 DEG C, and displaying the generation of the sponge metallic titanium through SEM (Scanning Electron Microscope) and XRD (X-Ray Diffraction) analysis after the electrolysis is carried out for two hours.
Description
Technical field:
The present invention relates to a kind of method of producing metal titanium, more particularly, relate to a kind of directly electrolytic reduction TiO of solid oxygen-ion membrane (som) (SOM) that utilizes
2Produce the method for sponge grease titanium; This method solved Prevent Carbon Contamination in the FFC method, current efficiency low, to problems such as ingredient requirement harshnesses.
Background technology:
Traditional metal titanium production method is magnesiothermy (a Kroll method), and this method complex process, cost height, energy consumption are big, seriously polluted, cause holding at high price of titanium or titanium alloy.The success of aluminium, magnesium eletrolysis method is imagined with electrolytic process people always and is realized producing cheaply continuously of metal titanium, but never success.At present, research focus about the electrolytic process of titanium is the FFC method, the proposition of this method has been opened up a new direction for electrolytic process prepares titanium sponge, but this method also exists fatal shortcoming: one is exactly that current efficiency is low, do anode owing to use graphite in this method, the ablation of graphite makes side reaction aggravation in the electrolytic process, even causes short circuit current; It two is exactly that current potential is wayward, TiO
2Itself be nonconducting, only when electrolysis begins, apply big voltage, make after the ionization of partial oxygen atom, could conduct electricity.CONTROLLED POTENTIAL guarantees that metal titanium separates out, and fused salt is not a difficult point by electrolysis.After the FFC method proposed, the various countries scholar successively studied this method, but all fails fundamentally to solve an above difficult problem.The SOM method is a kind of novel process of utilizing solid oxygen-ion membrane (som) to prepare metal, and principle as shown in Figure 1.This method has prepared at electrolytic oxidation magnesium and has obtained success on the magnesium.Metal oxide is dissolved in the molten salt electrolyte, under voltage control, oxonium ion and metal ion directional migration, reach the purpose of preparation metal, for the preparation metal titanium, it is infeasible directly using this method, and difficulty is present in following 2 points, the one, fail to find a kind of fine dissolving TiO so far
2Fused salt, be exactly that Ti has the multivalence attitude in addition, disperse will reduce current efficiency greatly in fused salt.
Summary of the invention:
The present invention is exactly at the problems referred to above, and a kind of method of producing the sponge grease titanium is provided; This method solved Prevent Carbon Contamination in the FFC method, current efficiency low, to the problem of ingredient requirement harshness.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and the method that the present invention adopts is: at 1150 ℃ MgF
2-CaF
2In the system, apply 3.2V voltage, electrolysis 2 hours, SEM, XRD analysis show the sponge grease titanium and generate.
Beneficial effect of the present invention:
Use the inventive method, at MgF
2-CaF
2In the molten salt system, promptly there is metal titanium to separate out in the short time at negative electrode.The proposition of this method is that a new direction has been opened up in the preparation of rare refractory metal.Many rare refractory metals have the fusing point height, the characteristics such as many of appraising at the current rate, thereby have determined that the hot reducing methods that adopt are produced more in the industrial production.Since hot reducing method have production process discontinuous, to shortcomings such as equipment requirements height, although cause these rare refractory metals very big at China's reserves, price is still high.Because these elements all have the multivalence attitude, make the fused salt electrolysis of " tradition " also be difficult to realize, because no matter be the metal-powder of the generation of disperse in fused salt, or multivalence attitude ion, all will reduce electrolytic efficiency greatly, the proposition of present method then can effectively solve an above difficult problem.
Embodiment:
The method that the present invention adopts is: at 1150 ℃ MgF
2-CaF
2In the system, apply 3.2V voltage, electrolysis 2 hours, SEM, XRD analysis show metal titanium and generate.
Described electrolysis raw material is chemical pure TiO
2(〉=98.0%); The ionogen fused salt constitutes 55.5wt%MgF
2-44.5wt%CaF
2Solid oxygen-ion membrane (som) be the stabilized with yttrium oxide that can purchase of market tubular zirconium-oxide (
); Whole process is to carry out electrolysis under the high-purity argon gas protection.
Heating unit is a siderochrome aluminum pipe formula process furnace; Adopt FP93 program temperature controller to carry out temperature control; The electrolysis direct supply is the adjustable D.C. regulated power supply of " LUYANG " YB1720A type.
Claims (3)
1. a method of producing metal titanium is characterized in that the MgF at 1150 ℃
2-CaF
2In the system, apply 3.2V voltage, electrolysis 2 hours, SEM, XRD analysis show the sponge grease titanium and generate.
2. a kind of method of producing metal titanium according to claim 1 is characterized in that described electrolysis raw material is chemical pure TiO
2(〉=98.0%); The ionogen fused salt constitutes 55.5wt%MgF
2-44.5wt%CaF
2
3. a kind of method of producing metal titanium according to claim 1 is characterized in that it being to carry out electrolysis under the high-purity argon gas protection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100130714A CN101994131A (en) | 2009-08-12 | 2009-08-12 | Method for producing metallic titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100130714A CN101994131A (en) | 2009-08-12 | 2009-08-12 | Method for producing metallic titanium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101994131A true CN101994131A (en) | 2011-03-30 |
Family
ID=43784868
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100130714A Pending CN101994131A (en) | 2009-08-12 | 2009-08-12 | Method for producing metallic titanium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101994131A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947874A (en) * | 2017-04-18 | 2017-07-14 | 北京科技大学 | A kind of method that two-step method prepares high purity titanium |
| CN108546964A (en) * | 2018-05-29 | 2018-09-18 | 钢研晟华科技股份有限公司 | A kind of preparation facilities and preparation method of Titanium |
| CN112981467A (en) * | 2021-02-04 | 2021-06-18 | 重庆大学 | Method for reducing carbon pollution in molten salt electrolysis process |
-
2009
- 2009-08-12 CN CN2009100130714A patent/CN101994131A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947874A (en) * | 2017-04-18 | 2017-07-14 | 北京科技大学 | A kind of method that two-step method prepares high purity titanium |
| CN106947874B (en) * | 2017-04-18 | 2018-11-27 | 北京科技大学 | A kind of method that two-step method prepares high purity titanium |
| CN108546964A (en) * | 2018-05-29 | 2018-09-18 | 钢研晟华科技股份有限公司 | A kind of preparation facilities and preparation method of Titanium |
| CN112981467A (en) * | 2021-02-04 | 2021-06-18 | 重庆大学 | Method for reducing carbon pollution in molten salt electrolysis process |
| CN112981467B (en) * | 2021-02-04 | 2024-01-26 | 重庆大学 | Method for reducing carbon pollution in molten salt electrolysis process |
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| C57 | Notification of unclear or unknown address | ||
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Addressee: Wang Xin Document name: Notification of Passing Preliminary Examination of the Application for Invention |
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Addressee: Cheng Simiao Document name: Notification of before Expiration of Request of Examination as to Substance |
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| DD01 | Delivery of document by public notice |
Addressee: Cheng Simiao Document name: Notification that Application Deemed to be Withdrawn |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20110330 |