CN103526050B - Production technology for welded pipe level sponge titanium - Google Patents
Production technology for welded pipe level sponge titanium Download PDFInfo
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- CN103526050B CN103526050B CN201310457493.7A CN201310457493A CN103526050B CN 103526050 B CN103526050 B CN 103526050B CN 201310457493 A CN201310457493 A CN 201310457493A CN 103526050 B CN103526050 B CN 103526050B
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Abstract
The invention discloses a production technology for welded pipe level sponge titanium and relates to the field of sponge titanium smelting and titanium material machining. According to the production technology, pure oxygen is used for oxidizing sponge titanium particles in a raw sponge titanium stage to realize oxygenation, so that the oxygen content of titanium welded pipes is more uniform, the yield of the titanium welded pipes can be greatly increased, the production cost of the titanium welded pipes is reduced, the technological level of the titanium welded pipe industry is improved, the integral development of the titanium industry of China is further promoted, the problem that high-end titanium materials depend on imports is solved thoroughly, and the development of the space and aeronautics industry in the high-end application field of the titanium welded pipes is further promoted; and meanwhile, according to the production technology, the content of other impurities can remain unchanged, the manufacturing requirements of the titanium welded pipes are met, and an oxygenation link in the titanium welded pipe machining process is effectively replaced, so that the problem of oxygenation segregation of the titanium welded pipes is solved thoroughly.
Description
[technical field]
The present invention relates to sponge titanium smelting and titanium material manufacture field, be specifically related to a kind of production technique of welded tube level titanium sponge.
[background technology]
Known, titanium welding pipe has that density is little, quality is light, without features such as magnetic are nontoxic, its intensity, hardness and high and low temperature resistance are excellent, and have good machining property, corrosion resistance nature, hydrogen storage property and heat exchange property, there is memory and supraconductivity simultaneously, so be widely used in the fields such as navigation, space flight, automobile, therapeutic physical education, electric power, chlor-alkali, sea water desaltination.
The at present development of external titanium welding pipe and the development of supporting utilisation technology ripe, but be in the blockade on new techniques phase, the technical development of China's titanium welded tube is also immature, every year still need from high-end titanium materials such as a large amount of titanium welding pipes of external import.Titanium welding pipe requires sufficiently high oxygen level and ensures its intensity and hardness, and require lower to other impurity components, the GB titanium sponge starting material produced according to a conventional method are difficult to ensure this requirement, therefore titanium welding pipe manufacturer adopts in fusion process to add the method oxygenation of pure TiO2 powder at present, but because pure TiO2 powder fusing point is high, easy generation segregation, is difficult to ensure its homogeneity, is one of key restriction factors of the domestic titanium welding pipe production technology development of impact.
Chinese patent, the applying date is on September 11st, 2012, publication number is the production technique disclosing high-oxygen sponge titanium in the patent of CN102816941, but this invention is in sponge titanium smelting process, by controlling the oxygen level in titanium tetrachloride, reach the object of oxygenation, its defect one is because in titanium sponge production process, produce the link of oxygen except titanium tetrachloride is brought into, still into oxygen level can be brought in follow-up reduction distillation process, and this oxygen level is wayward, it controls a link simultaneously, therefore effectively can not control the oxygen level of Sponge Titanium; Two is improve the oxygen level in titanium tetrachloride, can cause the rising of other foreign matter contents simultaneously, because the oxygen in titanium tetrachloride is not Individual existence, mainly exist with the form of compound, and as VOCl3, as improved oxygen level, other impurity can improve simultaneously, as V etc.
[summary of the invention]
In order to overcome the deficiency of above-mentioned technology, the invention provides a kind of production technique of welded tube level titanium sponge, the present invention is by realizing oxygenation in the starting material titanium sponge stage by adopting pure oxygen oxidation titanium sponge particles, make the oxygen level of titanium welding pipe evenly, greatly can promote the qualification rate of titanium welding pipe, reduce its production cost, improve the state of the art of titanium welding pipe industry, and then driven the overall development of China's titanium industry, thoroughly will solve high-end titanium material dependence on import problem, promote the development of titanium welding pipe high-end applications field aerospace further.
For realizing goal of the invention as above, the present invention adopts technical scheme as described below:
A production technique for welded tube level titanium sponge, described production technique specifically comprises the steps:
The first step, charging: in area in preparation, load titanium sponge particles in oxidation reactor, and by oxidation reactor sealing cover lid on oxidation reactor;
Second step, oxidation reactor to be vacuumized: by vacuum system, oxidation reactor is evacuated to below 25Pa;
3rd step, to oxygenation in oxidation reactor: oxygenation capacity oxidation after titanium sponge re-set target content and oxidation before titanium sponge oxygen level calculate;
4th step, heated oxide: be incubated 1 ~ 3 hour after process furnace being warming up to 500 ~ 700 DEG C, stop heating, promotes oxygen and titanium sponge reaction by heating;
5th step, argon-filled protection: object is after oxidation terminates, for avoiding into air, nitrogen content increases, with argon shield;
6th step, take out titanium sponge after cooling;
7th step, inspection: titanium sponge is tested.
The production technique of described welded tube level titanium sponge, described vacuum system is vacuum pump.
The production technique of described welded tube level titanium sponge, 0.1kg high purity oxygen gas, under gas meter controls, is once passed into oxidation reactor by the inflation inlet that oxidation reactor sealing cover is arranged with oxygen cylinder by described oxygenation capacity, starts heating after 5 ~ 20 minutes.
The production technique of described welded tube level titanium sponge, oxidation reactor is evacuated to below 25Pa by the mouth of finding time be arranged on oxidation reactor sealing cover by described vacuum system.
The production technique of described welded tube level titanium sponge, during described argon-filled protection, by being arranged on inflation inlet on oxidation reactor sealing cover toward applying argon gas in oxidation reactor.
The production technique of described welded tube level titanium sponge, adopts water-cooled during described cooling, takes out titanium sponge after being cooled to normal temperature.
Adopt technical scheme as above, the present invention has superiority as described below:
The production technique of a kind of welded tube level titanium sponge of the present invention, the present invention is by realizing oxygenation in the starting material titanium sponge stage by adopting pure oxygen oxidation titanium sponge particles, make the oxygen level of titanium welding pipe evenly, greatly can promote the qualification rate of titanium welding pipe, reduce its production cost, improve the state of the art of titanium welding pipe industry, and then driven the overall development of China's titanium industry, thoroughly will solve high-end titanium material dependence on import problem, the development of further promotion titanium welding pipe high-end applications field aerospace, the present invention simultaneously can realize other foreign matter contents and remain unchanged, meet the making requirement of titanium welding pipe, effectively instead of the oxygenation link in the titanium welding pipe course of processing, thoroughly solve titanium welding pipe oxygenation segregation problems.
[accompanying drawing explanation]
Fig. 1 is the structural representation of present invention process equipment;
In the drawings: 1, process furnace; 2, oxidation reactor; 3, oxidation reactor sealing cover; 4, to find time mouth; 5, inflation inlet; 6, titanium sponge particles.
[embodiment]
Can explain the present invention in more detail by the following examples, the present invention is not limited to the following examples;
The production technique of a kind of welded tube level titanium sponge of the present invention, described production technique specifically comprises the steps:
The first step, charging: in area in preparation, load titanium sponge particles 6 in oxidation reactor 2, and cover on oxidation reactor 2 by oxidation reactor sealing cover 3;
Second step, oxidation reactor 2 to be vacuumized: by vacuum system, oxidation reactor 2 is evacuated to below 25Pa, oxidation reactor 2 is evacuated to below 25Pa by the mouth 4 of finding time be arranged on oxidation reactor sealing cover 3 by described vacuum system, wherein vacuum system is vacuum pump
3rd step, to oxygenation in oxidation reactor 2: oxygenation capacity oxidation after titanium sponge re-set target content and oxidation before titanium sponge oxygen level calculate, described oxygenation capacity is under gas meter controls, once 0.1kg high purity oxygen gas is passed into oxidation reactor 2 by the inflation inlet 5 that oxidation reactor sealing cover 3 is arranged with oxygen cylinder, after 5 ~ 20 minutes, start heating;
4th step, heated oxide: be incubated 1 ~ 3 hour after process furnace 1 is warming up to 500 ~ 700 DEG C, stop heating, promotes oxygen and titanium sponge reaction by heating;
5th step, argon-filled protection: object is after oxidation terminates, for avoiding into air, nitrogen content increases, with argon shield, during described argon-filled protection, by being arranged on inflation inlet 5 on oxidation reactor sealing cover 3 toward applying argon gas in oxidation reactor 2;
6th step, take out titanium sponge after cooling, adopt water-cooled during described cooling, after being cooled to normal temperature, take out titanium sponge;
7th step, inspection: titanium sponge is tested.
Specific embodiments of the invention:
It should be noted that: for a person skilled in the art; under the prerequisite not departing from the inventive method; process furnace and the oxidation reactor of multi-form differing capacities can also be adopted; adopt different oxygenation modes; different Heating temperatures, soaking time etc. handle processing parameter etc.; once make the welded tube level Sponge Titanium of different oxygen, Different Weight, all belong to protection scope of the present invention.
Embodiment 1
100kg titanium sponge is oxidized
The first step: material prepares, prepares 100kg 0 grade of titanium sponge, its chemical composition as;
The test of 100kg0 level titanium sponge chemical composition and hardness
Second step: equipment prepares: process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
3rd step: test is implemented
Charging: in area in preparation, loads in oxidation reactor 2 by test 100kg0 level titanium sponge;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is loaded in process furnace 1;
Oxygenation: under gas meter controls, once 0.1kg high purity oxygen gas is passed into oxidation reactor 2 with oxygen cylinder, starts heating after 10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 DEG C, stops heating;
Argon-filled protection: heat complete, argon filling is to 0.025MPa;
Cooling is taken out: adopt water-cooled, take out after being cooled to normal temperature;
Inspection by sampling, shown in assay following table:
100kg0 level Sponge Titanium oxidation results
4th step: effect analysis
On titanium sponge composition after this oxidation shown in table, O content reaches 0.125%, and compared with before oxidation, other impurity components are without considerable change, and oxidation effectiveness is good.
Embodiment 2
1000kg titanium sponge is oxidized
The first step: material prepares, prepares 1000kg 1 grade of titanium sponge, its chemical composition as;
1000kg 1 grade test titanium sponge chemical composition and hardness
Second step: equipment prepares, process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
3rd step: test is implemented
Charging: in area in preparation, loads in oxidation reactor 2 by test 1000kg 1 grade of titanium sponge;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is loaded in process furnace 1;
Oxygenation: under gas meter controls, once 0.7kg high purity oxygen gas is passed into oxidation reactor 2 with oxygen cylinder, starts heating after 10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 DEG C, stops heating;
Argon-filled protection: heat complete, argon filling is to 0.025MPa;
Cooling is taken out: adopt water-cooled, take out after being cooled to normal temperature;
Inspection by sampling, assay is as shown in the table:
1000kg1 level Sponge Titanium oxidation results
4th step: effect analysis
As shown above, O content reaches 0.132% to titanium sponge composition after this oxidation, and compared with before oxidation, other impurity components are without considerable change, and oxidation effectiveness is good.
Embodiment 3
2000kg titanium sponge is oxidized
The first step: material prepares, prepares 2000kg 0 grade of titanium sponge, its chemical composition as;
2000kg 0 grade test titanium sponge chemical composition and hardness
Second step: equipment prepares, process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
3rd step: test is implemented
Charging: in area in preparation, loads in oxidation reactor 2 by test 2000kg 0 grade of titanium sponge;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is loaded in process furnace 1;
Oxygenation: under gas meter controls, once 1.5kg high purity oxygen gas is passed into oxidation reactor 2 with oxygen cylinder, starts heating after 10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 DEG C, stops heating;
Argon-filled protection: heat complete, argon filling is to 0.025MPa;
Cooling is taken out: adopt water-cooled, take out after being cooled to normal temperature;
Inspection by sampling, assay is as shown in the table:
2000kg 0 grade of titanium sponge oxidation results
4th step: effect analysis
As shown above, O content reaches 0.118% to titanium sponge composition after this oxidation, and compared with before oxidation, other compositions are without considerable change, and oxidation effectiveness is good.
In sum, oxygen level of the present invention has met the requirement of titanium welding pipe, titanium welding pipe is produced and is adopted this product, the oxygenation link in production process can be cut, the unacceptable product amount brought due to oxygenation segregation is at present made to reduce to zero, substantially increase the accepted product percentage of titanium welding pipe, reduce its production cost, make China's titanium Welded tube production technology obtain epoch-making lifting.
Part not in the detailed description of the invention is prior art.
The embodiment selected in this article in order to open object of the present invention, currently thinks to be suitable for, but it is to be understood that the present invention is intended to comprise all changes belonging to the embodiment in this design and invention scope and improvement.
Claims (6)
1. a production technique for welded tube level titanium sponge, is characterized in that: described production technique specifically comprises the steps:
The first step, charging: in area in preparation, load titanium sponge particles (6) in oxidation reactor (2), and by oxidation reactor sealing cover (3) lid to oxidation reactor (2);
Second step, oxidation reactor (2) to be vacuumized: by vacuum system, oxidation reactor (2) is evacuated to below 25Pa;
3rd step, to oxidation reactor (2) interior oxygenation: oxygenation capacity oxidation after titanium sponge re-set target content and oxidation before titanium sponge oxygen level calculate;
4th step, heated oxide: be incubated 1 ~ 3 hour after process furnace (1) is warming up to 500 ~ 700 DEG C, stop heating, promotes oxygen and titanium sponge reaction by heating;
5th step, argon-filled protection: object is after oxidation terminates, for avoiding into air, nitrogen content increases, with argon shield;
6th step, take out titanium sponge after cooling;
7th step, inspection: titanium sponge is tested.
2. the production technique of welded tube level titanium sponge according to claim 1, is characterized in that: described vacuum system is vacuum pump.
3. the production technique of welded tube level titanium sponge according to claim 1, it is characterized in that: described oxygenation capacity is under gas meter controls, once 0.1kg high purity oxygen gas is passed into oxidation reactor (2) by the upper inflation inlet (5) arranged of oxidation reactor sealing cover (3) with oxygen cylinder, after 5 ~ 20 minutes, start heating.
4. the production technique of welded tube level titanium sponge according to claim 1, is characterized in that: oxidation reactor (2) is evacuated to below 25Pa by the mouth of finding time (4) be arranged on oxidation reactor sealing cover (3) by described vacuum system.
5. the production technique of welded tube level titanium sponge according to claim 1, is characterized in that: during described argon-filled protection, by being arranged on past oxidation reactor (2) the interior applying argon gas of inflation inlet (5) on oxidation reactor sealing cover (3).
6. the production technique of welded tube level titanium sponge according to claim 1, is characterized in that: adopt water-cooled during described cooling, take out titanium sponge after being cooled to normal temperature.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103820654B (en) * | 2014-02-25 | 2015-08-12 | 洛阳双瑞精铸钛业有限公司 | A kind of devices and methods therefor to titanium sponge even oxygen aeration |
| CN104772468A (en) * | 2015-03-27 | 2015-07-15 | 洛阳双瑞精铸钛业有限公司 | Heating oxidation oxygenation method of titanium sponge for TA2-grade welded pipe |
Citations (7)
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| JP2003089829A (en) * | 2001-09-19 | 2003-03-28 | Toho Titanium Co Ltd | Method for producing high-oxygen titanium |
| JP2008200695A (en) * | 2007-02-19 | 2008-09-04 | Osaka Titanium Technologies Co Ltd | Method for manufacturing high oxygen titanium ingot |
| CN101517103A (en) * | 2006-09-25 | 2009-08-26 | 埃尔温斯·布卢姆伯格斯 | Method and apparatus for continuous producing of metallic titanium and titanium-based alloys |
| CN101613825A (en) * | 2003-10-18 | 2009-12-30 | 攀枝花金钛高科技有限责任公司 | The method of utilizing titanium, iron ore to produce titanium, steel work |
| CN102181670A (en) * | 2011-04-25 | 2011-09-14 | 东北大学 | Method for preparing titanium sponge through magnesium and chlorine recycling |
| CN102816941A (en) * | 2012-09-11 | 2012-12-12 | 朝阳金达钛业有限责任公司 | Process and device for producing high-oxygen sponge titanium |
| CN103740951A (en) * | 2013-12-26 | 2014-04-23 | 攀钢集团钛业有限责任公司 | Treatment method of standard exceeding of content of chlorine in titanium sponge |
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- 2013-09-30 CN CN201310457493.7A patent/CN103526050B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003089829A (en) * | 2001-09-19 | 2003-03-28 | Toho Titanium Co Ltd | Method for producing high-oxygen titanium |
| CN101613825A (en) * | 2003-10-18 | 2009-12-30 | 攀枝花金钛高科技有限责任公司 | The method of utilizing titanium, iron ore to produce titanium, steel work |
| CN101517103A (en) * | 2006-09-25 | 2009-08-26 | 埃尔温斯·布卢姆伯格斯 | Method and apparatus for continuous producing of metallic titanium and titanium-based alloys |
| JP2008200695A (en) * | 2007-02-19 | 2008-09-04 | Osaka Titanium Technologies Co Ltd | Method for manufacturing high oxygen titanium ingot |
| CN102181670A (en) * | 2011-04-25 | 2011-09-14 | 东北大学 | Method for preparing titanium sponge through magnesium and chlorine recycling |
| CN102816941A (en) * | 2012-09-11 | 2012-12-12 | 朝阳金达钛业有限责任公司 | Process and device for producing high-oxygen sponge titanium |
| CN103740951A (en) * | 2013-12-26 | 2014-04-23 | 攀钢集团钛业有限责任公司 | Treatment method of standard exceeding of content of chlorine in titanium sponge |
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