CN103526050A - Production technology for welded pipe level sponge titanium - Google Patents
Production technology for welded pipe level sponge titanium Download PDFInfo
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- CN103526050A CN103526050A CN201310457493.7A CN201310457493A CN103526050A CN 103526050 A CN103526050 A CN 103526050A CN 201310457493 A CN201310457493 A CN 201310457493A CN 103526050 A CN103526050 A CN 103526050A
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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 good, and there are good machining property, corrosion resistance nature, hydrogen storage property and heat exchange property, there is memory and supraconductivity, so be widely used in the fields such as navigation, space flight, automobile, therapeutic physical education, electric power, chlor-alkali, sea water desaltination simultaneously.
The development of at present external titanium welding pipe and the development of supporting utilisation technology are ripe, but in the blockade on new techniques phase, the technical development of China's titanium welded tube is also immature, every year still need be from a large amount of high-end titanium materials such as titanium welding pipe of external import.Titanium welding pipe requires have sufficiently high oxygen level to guarantee its intensity and hardness, and require lower to other impurity components, the GB titanium sponge starting material of producing are according to a conventional method difficult to guarantee 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, easily producing segregation, be difficult to guarantee 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 in the patent of CN102816941, to disclose the production technique of hyperoxia titanium sponge, 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, in follow-up reduction distillation process, still can bring oxygen level into, and this oxygen level is wayward, it controls a link simultaneously, therefore can not effectively control the oxygen level of Sponge Titanium; The 2nd, 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, be mainly that the form with compound exists, 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 to be oxidized titanium sponge particle, make the oxygen level of titanium welding pipe more even, can greatly 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, to thoroughly solve high-end titanium material dependence on import problem, further promote the development of titanium welding pipe high-end applications field aerospace.
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, titanium sponge particle is packed in oxidation reactor, and oxidation reactor sealing cover is covered on oxidation reactor;
Second step, oxidation reactor is vacuumized: by vacuum system, oxidation reactor is evacuated to below 25Pa;
The 3rd step, to oxygenation in oxidation reactor: oxygenation capacity calculates by titanium sponge oxygen level before titanium sponge re-set target content after oxidation and oxidation;
The 4th step, heated oxide: after process furnace is warming up to 500～700 ℃, be incubated 1～3 hour, stop heating, by heating, promote oxygen and titanium sponge to react;
The 5th step, argon-filled protection: object is after oxidation finishes, for avoiding into air, nitrogen content increases, with argon shield;
The 6th step, take out titanium sponge after cooling;
The 7th step, check: 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, described oxygenation capacity, under gas meter is controlled, once passes into oxidation reactor by 0.1kg high purity oxygen gas by the inflation inlet arranging on oxidation reactor sealing cover with oxygen cylinder, starts heating after 5～20 minutes.
The production technique of described welded tube level titanium sponge, described vacuum system is evacuated to oxidation reactor below 25Pa by the mouth of finding time being arranged on oxidation reactor sealing cover.
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, describedly adopts water-cooled when 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 to be oxidized titanium sponge particle, make the oxygen level of titanium welding pipe more even, can greatly 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, to thoroughly solve high-end titanium material dependence on import problem, further promote the development of titanium welding pipe high-end applications field aerospace, the present invention simultaneously can realize other foreign matter contents and remain unchanged, met the making requirement of titanium welding pipe, effectively substituted the oxygenation link in the titanium welding pipe course of processing, thoroughly solved titanium welding pipe oxygenation segregation problem.
[accompanying drawing explanation]
Fig. 1 is the structural representation of processing unit of the present invention;
In the drawings: 1, process furnace; 2, oxidation reactor; 3, oxidation reactor sealing cover; 4, the mouth of finding time; 5, inflation inlet; 6, titanium sponge particle.
[embodiment]
By the following examples, can explain in more detail the present invention, 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, titanium sponge particle 6 is packed in oxidation reactor 2, and oxidation reactor sealing cover 3 is covered to oxidation reactor 2;
Second step, oxidation reactor 2 is vacuumized: by vacuum system, oxidation reactor 2 is evacuated to below 25Pa, described vacuum system is evacuated to oxidation reactor 2 below 25Pa by the mouth 4 of finding time being arranged on oxidation reactor sealing cover 3, wherein vacuum system is vacuum pump
The 3rd step, to the interior oxygenation of oxidation reactor 2: oxygenation capacity calculates by titanium sponge oxygen level before titanium sponge re-set target content after oxidation and oxidation, described oxygenation capacity is under gas meter is controlled, with oxygen cylinder, once 0.1kg high purity oxygen gas is passed into oxidation reactor by the inflation inlet 5 arranging on oxidation reactor sealing cover 3 and after 2,5～20 minutes, start heating;
The 4th step, heated oxide: after process furnace 1 is warming up to 500～700 ℃, be incubated 1～3 hour, stop heating, by heating, promote oxygen and titanium sponge to react;
The 5th step, argon-filled protection: object is after oxidation finishes, 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 the interior applying argon gas of oxidation reactor 2;
The 6th step, take out titanium sponge after cooling, describedly adopt water-cooled when cooling, take out titanium sponge after being cooled to normal temperature;
The 7th step, check: titanium sponge is tested.
Specific embodiments of the invention:
It should be noted that: for a person skilled in the art; do not departing under the prerequisite of the inventive method; can also adopt process furnace and the oxidation reactor of multi-form differing capacities; adopt different oxygenation modes; different Heating temperatures, soaking time etc. are handled processing parameter etc.; the welded tube level Sponge Titanium of once making different oxygen, Different Weight, all belongs to protection scope of the present invention.
Embodiment 1
The oxidation of 100kg titanium sponge
The first step: material is prepared, prepares 0 grade of titanium sponge of 100kg, its chemical composition as;
100kg0 level is titanium sponge chemical composition and hardness for test
Second step: equipment is prepared: process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
The 3rd step: test is implemented
Charging: in area in preparation, test is packed in oxidation reactor 2 with 100kg0 level titanium sponge;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is packed in process furnace 1;
Oxygenation: under gas meter is controlled, once 0.1kg high purity oxygen gas is passed into oxidation reactor with oxygen cylinder and start heating after 2,10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 ℃, stop heating;
Argon-filled protection: heat completely, argon filling is to 0.025MPa;
Cooling taking-up: 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
The 4th step: effect analysis
This oxidation after titanium sponge composition on table shown in, O content reaches 0.125%, with oxidation before compare, other impurity components are without considerable change, oxidation effectiveness is good.
Embodiment 2
The oxidation of 1000kg titanium sponge
The first step: material is prepared, prepares 1 grade of titanium sponge of 1000kg, its chemical composition as;
1000kg is titanium sponge chemical composition and hardness for 1 grade of test
Second step: equipment is prepared, process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
The 3rd step: test is implemented
Charging: in area in preparation, test is packed in oxidation reactor 2 with 1 grade of titanium sponge of 1000kg;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is packed in process furnace 1;
Oxygenation: under gas meter is controlled, once 0.7kg high purity oxygen gas is passed into oxidation reactor with oxygen cylinder and start heating after 2,10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 ℃, stop heating;
Argon-filled protection: heat completely, argon filling is to 0.025MPa;
Cooling taking-up: 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
The 4th step: effect analysis
This oxidation after titanium sponge composition as shown above, O content reaches 0.132%, with oxidation before compare, other impurity components are without considerable change, oxidation effectiveness is good.
Embodiment 3
The oxidation of 2000kg titanium sponge
The first step: material is prepared, prepares 0 grade of titanium sponge of 2000kg, its chemical composition as;
2000kg is titanium sponge chemical composition and hardness for 0 grade of test
Second step: equipment is prepared, process furnace 1, oxidation reactor 2, oxidation reactor sealing cover 3 and matched with vacuum system etc.;
The 3rd step: test is implemented
Charging: in area in preparation, test is packed in oxidation reactor 2 with 0 grade of titanium sponge of 2000kg;
Find time: by vacuum system, above-mentioned oxidation reactor 2 is evacuated to below 25Pa, after oxidation reactor 2 is packed in process furnace 1;
Oxygenation: under gas meter is controlled, once 1.5kg high purity oxygen gas is passed into oxidation reactor with oxygen cylinder and start heating after 2,10 minutes;
Heated oxide: be incubated 2 hours after process furnace 1 is warming up to 600 ℃, stop heating;
Argon-filled protection: heat completely, argon filling is to 0.025MPa;
Cooling taking-up: adopt water-cooled, take out after being cooled to normal temperature;
Inspection by sampling, assay is as shown in the table:
0 grade of titanium sponge oxidation results of 2000kg
The 4th step: effect analysis
This oxidation after titanium sponge composition as shown above, O content reaches 0.118%, with oxidation before compare, other compositions are without considerable change, 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, can cut the oxygenation link in production process, make the unacceptable product amount of bringing due to oxygenation segregation at present reduce to zero, greatly improved the accepted product percentage of titanium welding pipe, reduced its production cost, made 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 selecting in this article in order to disclose object of the present invention, currently thinks suitablely, still, will be appreciated that, the present invention is intended to comprise that all belong to all changes and the improvement of the embodiment in this design and invention scope.
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, titanium sponge particle (6) is packed in oxidation reactor (2), and oxidation reactor sealing cover (3) lid is arrived on oxidation reactor (2);
Second step, oxidation reactor (2) is vacuumized: by vacuum system, oxidation reactor (2) is evacuated to below 25Pa;
The 3rd step, to the interior oxygenation of oxidation reactor (2): oxygenation capacity calculates by titanium sponge oxygen level before titanium sponge re-set target content after oxidation and oxidation;
The 4th step, heated oxide: after process furnace (1) is warming up to 500～700 ℃, be incubated 1～3 hour, stop heating, by heating, promote oxygen and titanium sponge to react;
The 5th step, argon-filled protection: object is after oxidation finishes, for avoiding into air, nitrogen content increases, with argon shield;
The 6th step, take out titanium sponge after cooling;
The 7th step, check: 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 is controlled, with oxygen cylinder, once 0.1kg high purity oxygen gas is passed into oxidation reactor (2) by the upper inflation inlet (5) arranging of oxidation reactor sealing cover (3), after 5～20 minutes, start heating.
4. the production technique of welded tube level titanium sponge according to claim 1, is characterized in that: described vacuum system is evacuated to oxidation reactor (2) below 25Pa by find time mouthful (4) that are arranged on oxidation reactor sealing cover (3).
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 the past interior applying argon gas of oxidation reactor (2) 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: describedly adopt water-cooled when cooling, take out titanium sponge after being cooled to normal temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820654A (en) * | 2014-02-25 | 2014-05-28 | 洛阳双瑞精铸钛业有限公司 | Uniform oxygenation device for titanium sponge and method thereof |
| 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 |
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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 |
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2013
- 2013-09-30 CN CN201310457493.7A patent/CN103526050B/en not_active Expired - Fee Related
Patent Citations (7)
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| 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 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820654A (en) * | 2014-02-25 | 2014-05-28 | 洛阳双瑞精铸钛业有限公司 | Uniform oxygenation device for titanium sponge and method thereof |
| 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 |
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