CN101497945A - Method for preparing low oxygen-containing metallic titanium - Google Patents
Method for preparing low oxygen-containing metallic titanium Download PDFInfo
- Publication number
- CN101497945A CN101497945A CNA2009103000873A CN200910300087A CN101497945A CN 101497945 A CN101497945 A CN 101497945A CN A2009103000873 A CNA2009103000873 A CN A2009103000873A CN 200910300087 A CN200910300087 A CN 200910300087A CN 101497945 A CN101497945 A CN 101497945A
- Authority
- CN
- China
- Prior art keywords
- titanium
- oxygen
- reaction
- containing metallic
- metal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses a method for preparing low oxygen-containing metal titanium, and relates to the technical field of metal smelting. The method uses oxygen-containing titanium hydride powder or oxygen-containing metal titanium powder as a titanium-containing raw material and has the core process that the oxygen-containing titanium and calcium are mixed and heated, so that the calcium is evaporated, and the calcium in the form of gas and the oxygen are combined to become calcium oxide; and after the reaction, the lower oxygen-containing metal titanium can be obtained after cooling, crushing, acid washing and drying. The method has simple process and can prepare low oxygen-containing metal titanium.
Description
Technical field
The present invention relates to the Metal smelting technical field, particularly a kind of with oxygen-containing metallic titanium or contain the method that the oxygen titanium hydride is the feedstock production low oxygen-containing metallic titanium.
Background technology
The oxygen level of metal titanium product is the important indicator of quality product, the oxygen level of existing metal titanium product depends primarily on the principle and the operant level of present employing production technique, quite a few contains the higher substandard products of oxygen inevitable by-product, has influenced the effect of producing greatly.Because the strong oxytropism of metal titanium itself makes the deoxygenation of high oxygen metal become comparatively difficult, the present industrial simple effective method that also do not have.
Summary of the invention
Problem to be solved by this invention provides a kind of with oxygen-containing metallic titanium or contain the method for preparing low oxygen-containing metallic titanium that the oxygen titanium hydride is a raw material.
For addressing the above problem, the method of this preparation low oxygen-containing metallic titanium can adopt and contain the oxygen titanium hydride powder or adopt the oxygen metal titanium valve as titaniferous materials, its core is with oxygen containing titanium and calcium Hybrid Heating, make the calcium evaporation be combined into calcium oxide with the form of gas and oxygen wherein, reaction is after overcooling, pulverize, obtain the lower metal titanium of oxygen level after acid solution washing and the drying.
Specifically, wherein adopt and contain the oxygen titanium hydride powder and be as the method for preparing low oxygen-containing metallic titanium of titaniferous materials:
To contain oxygen titanium hydride powder and calcium metal in airtight reaction vessel internal heating to 700 ℃～1000
℃React, allow titanium hydride powder be decomposed into metal titanium and hydrogen, extract hydrogen and other foreign gas in the described reaction vessel out, allow the calcium metal evaporation be combined into calcium oxide with oxygen, reaction obtains metal titanium after overcooling is pulverized after acid solution washing and the drying.
Above-mentionedly thisly prepare in the scheme of low oxygen-containing metallic titanium as titaniferous materials to contain the oxygen titanium hydride powder, reaction times is according to the amount of reactant, the height of temperature of reaction is different and different, the amount of reactant is big more, temperature of reaction is low more, and then to need to finish time of reaction long more, otherwise the time that need finish reaction is short more, during industrial applications, be 700 in temperature of reaction
℃～1000
℃Condition under, the reaction times was generally 3～8 hours, was 780 in temperature of reaction
℃～920
℃Condition under, the reaction times was advisable with 3～4 hours.
Wherein adopt the oxygen metal titanium valve to be as the method for preparing low oxygen-containing metallic titanium of titaniferous materials:
With oxygen metal titanium valve and calcium metal at airtight reaction vessel internal heating to 700
℃～1000
℃React, by the gas in the described reaction vessel of reaction consumes, allow the calcium metal evaporation be combined into calcium oxide with oxygen, reaction obtains the lower metal titanium of oxygen level after overcooling is pulverized after acid solution washing and the drying.
Above-mentioned thisly prepare as titaniferous materials in the scheme of low oxygen-containing metallic titanium with the oxygen metal titanium valve, described temperature of reaction is general 780
℃～920
℃, the reaction times is according to the amount of reactant, and the height of temperature of reaction is different, and the amount of reactant is big more and different, and temperature of reaction is low more, and then to need to finish time of reaction long more, on the contrary the time that need finish reaction is short more, during industrial applications, is being 700 in temperature of reaction
℃～1000
℃Condition under, the reaction times was generally 3～8 hours, was 780 in temperature of reaction
℃～920
℃Condition under, the reaction times was advisable with 3～4 hours.
Owing to adopted such scheme, not only technology is simple for this method for preparing low oxygen-containing metallic titanium of the present invention, and can obtain the very low metal titanium of oxygen level.
Embodiment
Table 1: correlation parameter and the result's (other foreign matter contents of raw material no increase trend after this art breading in the result of implementation) of five embodiment who with the oxygen metal titanium valve is the method for preparing low oxygen-containing metallic titanium of titaniferous materials
| Embodiment | Titaniferous materials | Titaniferous materials weight (gram) | Titaniferous materials titanium content (%) | Titaniferous materials oxygen level (%) | Calcium metal consumption (gram) | Temperature of reaction (℃) | Reaction times (hour) | Product weight (gram) | Product titanium content (%) | Product oxygen level (%) |
| 1 | Metallic titanium powder | 100 | 95.0 | 4.22 | 27 | 1000 | 3 | 86.2 | 98.1 | 0.63 |
| 2 | Metallic titanium powder | 100 | 95.0 | 4.22 | 27 | 920 | 3 | 85.6 | 98.6 | 0.59 |
| 3 | Metallic titanium powder | 100 | 96.6 | 2.56 | 16 | 850 | 3.5 | 88.8 | 98.7 | 0.44 |
| 4 | Metallic titanium powder | 100 | 97.3 | 1.89 | 12 | 780 | 4 | 90.4 | 98.8 | 0.38 |
| 5 | Metallic titanium powder | 100 | 97.3 | 1.89 | 12 | 700 | 8 | 90.2 | 98.6 | 0.40 |
The working method step of embodiment 1～5 is as follows:
1, reaction among table 1 embodiment is required oxygen metal titanium valve is by 100 mesh standard sieves.
2, under argon shield, the metallic titanium powder of sieving is mixed with calcium metal among table 1 embodiment, in the reaction vessel of packing into then, get rid of the air in the reaction vessel, the outlet of closed reaction vessel.
3, reaction vessel is heated to temperature of reaction among table 1 embodiment, insulation reaches the reaction times among table 1 embodiment.Allow calcium metal and oxygen be combined into calcium oxide, in the time of reaction, air and calcium metal reaction remaining in the reaction vessel are complete, form negative pressure in the reaction vessel, calcium is evaporated under temperature of reaction be combined into calcium oxide with gasiform form and oxygen.
4, reaction vessel is cooled to normal temperature, under argon shield, the resultant of reaction material is taken out and be crushed to 100 orders.
5, the resultant of reaction after will pulverizing adds in the dilute hydrochloric acid solution and carries out previous cleaning, again with the dilute sulphuric acid washing once.
6, will wash thing through vacuum-drying, obtain low oxygen-containing metallic titanium.
Table 2: to contain correlation parameter and the result's (other foreign matter contents of raw material no increase trend after this art breading in the result of implementation) of five embodiment that the oxygen titanium hydride powder is the method for preparing low oxygen-containing metallic titanium of titaniferous materials
| Embodiment | Titaniferous materials | Titaniferous materials weight (gram) | Titaniferous materials titanium content (%) | Titaniferous materials oxygen level (%) | Calcium metal consumption (gram) | Temperature of reaction (℃) | Reaction times (hour) | Product weight (gram) | Product titanium content (%) | Product oxygen level (%) |
| 6 | Titanium hydride powder | 100 | 94.0 | 3.22 | 20 | 1000 | 3 | 82.8 | 98.5 | 0.29 |
| 7 | Titanium hydride powder | 100 | 94.0 | 3.22 | 20 | 920 | 3 | 83.0 | 98.8 | 0.26 |
| 8 | Titanium hydride powder | 100 | 95.4 | 1.82 | 11 | 850 | 3.5 | 85.2 | 99.0 | 0.18 |
| 9 | Titanium hydride powder | 100 | 96.0 | 1.24 | 8 | 780 | 4 | 87.0 | 99.0 | 0.15 |
| 10 | Titanium hydride powder | 100 | 96.0 | 1.24 | 8 | 700 | 8 | 86.8 | 99.2 | 0.19 |
The working method step of embodiment 6～10 is as follows:
1, reaction among table 2 embodiment is the required oxygen titanium hydride powder that contains passes through 100 mesh standard sieves.
2, under argon shield, the titanium hydride powder that sieves is mixed the reaction vessel inner sealing reaction vessel of packing into then with calcium metal among table 2 embodiment.
3, in the gas in extracting reaction vessel out reaction vessel is heated to temperature of reaction among table 2 embodiment, insulation reaches the reaction times among table 2 embodiment.Calcium is evaporated under temperature of reaction be combined into calcium oxide with gasiform form and oxygen.
4, reaction vessel is cooled to normal temperature, under argon shield, the resultant of reaction material is taken out and be crushed to 100 orders.
5, the resultant of reaction after will pulverizing adds in the dilute hydrochloric acid solution and carries out previous cleaning, again with the dilute sulphuric acid washing once.
6, will wash thing through vacuum-drying, obtain low oxygen-containing metallic titanium.
Claims (6)
- [claim 1] a kind of method for preparing low oxygen-containing metallic titanium, it is characterized in that: will contain oxygen titanium hydride powder and calcium metal and react airtight reaction vessel internal heating to 700 ℃～1000 ℃, allow titanium hydride powder be decomposed into metal titanium and hydrogen, extract hydrogen and other foreign gas in the described reaction vessel out, allow the calcium metal evaporation be combined into calcium oxide with oxygen, reaction obtains metal titanium after overcooling is pulverized after acid solution washing and the drying.
- [claim 2] method for preparing low oxygen-containing metallic titanium according to claim 1 is characterized in that: described temperature of reaction is 780 ℃～920 ℃.
- [claim 3] method for preparing low oxygen-containing metallic titanium according to claim 1 and 2 is characterized in that: the described reaction times is 3～8 hours.
- [claim 4] a kind of method for preparing low oxygen-containing metallic titanium, it is characterized in that: oxygen metal titanium valve and calcium metal are reacted airtight reaction vessel internal heating to 700 ℃～1000 ℃, by the gas in the described reaction vessel of reaction consumes, allow the calcium metal evaporation be combined into calcium oxide with oxygen, reaction is after overcooling, pulverize, obtain the lower metal titanium of oxygen level after acid solution washing and the drying.
- [claim 5] method for preparing low oxygen-containing metallic titanium according to claim 4 is characterized in that: described temperature of reaction is 780 ℃～920 ℃.
- [claim 6] according to claim 4 or the 5 described methods that prepare low oxygen-containing metallic titanium, it is characterized in that: the described reaction times is 3～8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103000873A CN101497945B (en) | 2009-01-06 | 2009-01-06 | Method for preparing low oxygen-containing metallic titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103000873A CN101497945B (en) | 2009-01-06 | 2009-01-06 | Method for preparing low oxygen-containing metallic titanium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101497945A true CN101497945A (en) | 2009-08-05 |
| CN101497945B CN101497945B (en) | 2011-01-05 |
Family
ID=40945215
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009103000873A Expired - Fee Related CN101497945B (en) | 2009-01-06 | 2009-01-06 | Method for preparing low oxygen-containing metallic titanium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101497945B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016528393A (en) * | 2013-08-19 | 2016-09-15 | ユニバーシティ・オブ・ユタ・リサーチ・ファウンデイション | Production of titanium products |
| CN112095021A (en) * | 2020-01-21 | 2020-12-18 | 有研工程技术研究院有限公司 | Method for deeply removing oxygen in metal titanium by using super-oxophilic metal-calcium synergistic method |
| US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
| CN112846223A (en) * | 2021-01-11 | 2021-05-28 | 交通运输部天津水运工程科学研究所 | Preparation method of high-purity spherical metal titanium powder for 3D printing |
-
2009
- 2009-01-06 CN CN2009103000873A patent/CN101497945B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016528393A (en) * | 2013-08-19 | 2016-09-15 | ユニバーシティ・オブ・ユタ・リサーチ・ファウンデイション | Production of titanium products |
| US10190191B2 (en) | 2013-08-19 | 2019-01-29 | University Of Utah Research Foundation | Producing a titanium product |
| US10689730B2 (en) | 2013-08-19 | 2020-06-23 | University Of Utah Research Foundation | Methods of producing a titanium product |
| CN112095021A (en) * | 2020-01-21 | 2020-12-18 | 有研工程技术研究院有限公司 | Method for deeply removing oxygen in metal titanium by using super-oxophilic metal-calcium synergistic method |
| US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
| CN112846223A (en) * | 2021-01-11 | 2021-05-28 | 交通运输部天津水运工程科学研究所 | Preparation method of high-purity spherical metal titanium powder for 3D printing |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101497945B (en) | 2011-01-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101157373B1 (en) | Method for producing high purity porous silica and silicon from rice husk | |
| CN101659403B (en) | Hydro-thermal synthesis process of phosphide | |
| CN101497945B (en) | Method for preparing low oxygen-containing metallic titanium | |
| CN101200306B (en) | Method for preparing titanium dioxide primary product | |
| AU2020103465A4 (en) | Method for preparing high-purity spherical ruthenium powder by microwave one-step method | |
| CN106631753B (en) | Method for producing gallic acid by using superfine gallnut powder | |
| CN106006597B (en) | One kind containing Fe by ferrophosphorus low temperature preparationxPO4The method of substance | |
| CN101214993B (en) | Preparation method for nanometer zinc oxide | |
| CN101624659B (en) | Method for preparing low-oxygen metal zirconium | |
| CN102391196A (en) | Method for synthesizing zinc cyanurate by adopting normal pressure method | |
| Rangari et al. | Preparation and microscopic characterization of biobased nanoparticles from natural waste materials | |
| CN103484703A (en) | Preparation method of tungsten carbide-titanium carbide solid solution | |
| CN101503763B (en) | Method for preparing low oxygen content metal vanadium | |
| CN103130284B (en) | Method for producing nickel carbonyl powder from nickel hydroxide | |
| CN103101960A (en) | Method for preparing high-purity low-chlorine electroplating-grade cupric oxide | |
| CN105923659B (en) | A kind of preparation method of LITHIUM BATTERY superfine sheet cobalt hydroxide | |
| CN107745132A (en) | A kind of method that iron oxide red prepares high-purity iron powder | |
| Ekwenna et al. | The production of bio-silica from agro-industrial wastes leached and anaerobically digested rice straws | |
| Dalvand et al. | A facile fabrication of NiO nanoparticles from spent Ni–Cd batteries | |
| CN107827096A (en) | A kind of method that autocatalytic cleavage prepares embedded bimetallic and three metal carbon onions | |
| CN113149061B (en) | Preparation method of superfine zinc oxide powder | |
| CN108408709A (en) | A kind of preparation process of pollution-free inexpensive iron manganese phosphate for lithium crystalline material | |
| CN104071799B (en) | A kind of talcum-magnetic metal nano composite material and preparation method thereof | |
| CN113415812A (en) | Preparation method and application of high-purity lithium sulfide | |
| CN102602940B (en) | Method for producing high-performance white carbon black and succinic acid by comprehensively utilizing white spirit lees |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110105 Termination date: 20160106 |