CN104999073A - Method and device for preparing high-purity and low-oxygen titanium powder through metal steam reduction - Google Patents
Method and device for preparing high-purity and low-oxygen titanium powder through metal steam reduction Download PDFInfo
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- CN104999073A CN104999073A CN201510421467.8A CN201510421467A CN104999073A CN 104999073 A CN104999073 A CN 104999073A CN 201510421467 A CN201510421467 A CN 201510421467A CN 104999073 A CN104999073 A CN 104999073A
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Abstract
The invention discloses a method and device for preparing high-purity and low-oxygen titanium powder through metal steam reduction. The method includes the steps that the method and device for preparing high-purity and low-oxygen titanium powder through metal steam reduction are adopted, active metal and titanium powder are put into a vacuum sealing heating furnace to carry out metal steam reduction so that high-purity titanium powder can be prepared; then washing, acid pickling and drying are conducted on the high-purity titanium powder to obtain the high-purity and low-oxygen titanium powder. The device comprises a furnace body provided with a furnace cavity. A hearth is arranged in the middle of the furnace cavity. A furnace pot is arranged in the hearth. A material frame is arranged in the furnace pot. A screen is installed on the material frame. A distance is reserved between the screen and the bottom of the furnace pot. The opening end of the top of the furnace pot is connected with a detachable furnace cover in a sealed mode. The furnace cover is provided with an exhaust valve, a pressure gauge and a vacuum pumping pipeline. The furnace pot is further connected with a gas inlet pipe. The method and device for preparing the high-purity and low-oxygen titanium powder through metal steam reduction have the advantages of being low in cost, high in efficiency, environmentally friendly, clean and the like.
Description
Technical field
The present invention relates to powder preparation technical field, be specifically related to method and device that high-purity low-oxygen titanium valve is prepared in the reduction of a kind of metal vapors.
Background technology
As a member of emerging metal, titanium has many outstanding characteristics, and as large in specific strength, proportion is little, corrosion-resistant, and pure titanium generally refers to the titanium material that purity is greater than 99%.High purity titanium has many excellent performances, the feature such as low in density, fusing point is high, intensity is low, plasticity is good, in recent years, along with the fast development of the high-tech industry such as Aero-Space, electronic information, the consumption of high purity titanium also gets more and more, how to prepare high purity titanium better, be the important directions of current Ti industry development.
The most frequently used method of the high-purity titanium valve of current preparation is mainly hydrogenation and dehydrogenization or atomization, but obtains the high titanium valve of purity through hydrogenation and dehydrogenization or atomization, and its oxygen content is higher, and the titanium valve that wherein hydrogenation and dehydrogenization obtains is irregularly shaped; And though the titanium valve that atomization obtains is for spherical, easily powder particle adhesion occurs in atomization process, powder size is bigger than normal and domain size distribution is very wide, therefore needs further to purify to obtain the titanium valve of high-purity low-oxygen.Such as, to adopt titanium sponge as raw material, preparing high-purity titanium valve by hydrogenation and dehydrogenization is example, because titanium sponge impurity content is higher, and with high temperature under very easily occur to be oxidized to form TiO
2introduce major impurity O element, the impurity content (especially oxygen content) of finally obtained titanium valve is higher, has had a strong impact on the performance of final obtained titanium valve, can not meet industrial requirements; Meanwhile, powder is also easily grown up and is lumpd in the high-temperature dehydrogenation stage, and therefore the purity of titanium valve and granularity are difficult to reach desirable degree, seriously constrain the development of powder metallurgy titanium industry.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency overcoming prior art existence, provides a kind of cost is low, efficiency is high, high-purity low-oxygen titanium valve is prepared in the reduction of the metal vapors of environment-protecting clean method and device.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A method for high-purity low-oxygen titanium valve is prepared in metal vapors reduction, it is characterized in that: comprise the following steps:
(1) choosing high-purity molten-salt electrolysis titanium is raw material, adopts hydrogenation and dehydrogenization or atomization to the obtained titanium valve of molten-salt electrolysis titanium processing;
(2) active metal identical for weight and titanium valve are placed in vacuum seal heating furnace, are heated to make active metal to form steam under vacuum conditions, the impurity generation reduction reaction in active metal steam and titanium valve obtains high-purity titanium valve; Wherein, the major impurity TiO in titanium valve
2be reduced, thus obtain high-purity Ti powder;
(3) high-purity titanium valve is washed, pickling and the dry metal oxide removing attachment, obtain high-purity low-oxygen titanium valve.
Above-mentioned method, preferably, is placed in vacuum seal heating furnace to titanium valve and active metal non-direct contact.In reduction process, titanium valve does not directly contact with active metal, and this kind of mode avoids the product pollution problem directly contacting and cause, and is beneficial to the content reducing impurity in product.
Above-mentioned method, preferably, in described step (2), active metal be prepared into particle be placed in material frame in vacuum seal heating furnace bottom, titanium valve is placed on the top of active metal particle by screen cloth.
Above-mentioned method, preferably, in described step (2), heating-up temperature is 1273 ~ 1290K, and temperature retention time is 2 ~ 3 hours, and the vacuum in described vacuum seal heating furnace is 3.3 × 10
-3pa ~ 8.2 × 10
-3pa.
Above-mentioned method, preferably, described active metal is Na, K, Ca, Li or Mg.
Above-mentioned method, preferably, the addition of described active metal and titanium valve is 50 ~ 60g.
Above-mentioned method, preferably, described HDH method comprises hydrogenation, ball milling and dehydrogenation three steps to the processing of molten-salt electrolysis titanium, specifically, first raw material is placed in the hydrogenation of hydrogenation and dehydrogenization stove and obtains titanium hydride particles, again titanium hydride particles ball mill crushing is obtained titanium hydride powders, then titanium hydride powders is placed in hydrogenation and dehydrogenization stove Oxidative Dehydrogenation and obtains titanium valve; Described atomization comprises inert gas atomizer method and rotating electrode atomized method to the processing of molten-salt electrolysis titanium.Wherein, namely inert gas atomizer method smashes metal liquid stream by high velocity air; Namely rotating electrode atomized method is made into pair of electrodes with metal or alloy, makes metal end face and arc contacts region become molten condition, then is thrown away by molten drop by the centrifugal force of High Rotation Speed, complete atomization process by electric discharge.
In the present invention, high-purity molten-salt electrolysis titanium is graininess.
As a total inventive concept, the present invention also provides a kind of device preparing high-purity low-oxygen titanium valve for metal vapors reduction, comprise the body of heater with furnace chamber, the middle part of described furnace chamber is provided with burner hearth, retort is provided with in described burner hearth, material frame is placed with in described retort, described material frame is equiped with screen cloth, spacing is left between described screen cloth and the bottom of retort, the open top end of described retort is sealedly connected with dismountable bell, described bell is provided with air bleeding valve, Pressure gauge and vacuum lead, and described retort is also connected with air inlet pipe.
Above-mentioned device, preferably, described bell is seal-installed on retort by hold down gag; Described air inlet pipe is provided with flowmeter.
Above-mentioned device, preferably, is filled with heat-preservation cotton between described burner hearth and inboard wall of furnace body.
Above-mentioned device, preferably, described body of heater, burner hearth, retort, material frame and bell are made by stainless steel.
Above-mentioned device, preferably, described screen surface is distributed with multiple circular pore, and this circular pore can make gas pass through and not allow titanium valve drop.
Above-mentioned device, preferably, described furnace cover lifting is completed by electronic screw lift, and housing by shaped steel and Plate Welding shaping, bell lining adopt fully fibrous structure, good heat insulating.
Above-mentioned device, when testing, is placed in material frame bottom by the active metal for generation of metal vapors, is reduced titanium valve and is placed on the screen cloth of material frame, then close bell, namely can be used for experiment.Start after extracting vacuum be heated to uniform temperature and be incubated a period of time, the metal vapors of generation by the pore of screen cloth be reduced titanium valve and contact, there is reduction reaction, thus avoid active metal and be reduced titanium valve and directly contact the product pollution problem caused.In addition; dismountable bell is connected with furnace sealing; serve the effect ensureing furnace sealing; avoid the gas effusion under sealing state; ensure that the inner enough pressure of burner hearth, thus guarantee that reduction reaction is correctly carried out efficiently, it also avoid furnace gas and to overflow the problem of environmental pollution caused; meanwhile, it also avoid the outer gas of stove and enter the reaction interference problem caused in stove.
Said apparatus is when testing, and along with the continuous rising of reaction temperature, the pressure of furnace gas constantly raises, concentration increases, be heated to uniform temperature and insulation process in, active metal steam can react with the reduced metal on screen cloth fully, guarantee reaction carry out efficiently.Whole device has the features such as intensity is high, reusable, structure is simple, cost is low, seal is excellent, method of operating is simple.
Compared with prior art, the invention has the advantages that: the method that high-purity low-oxygen titanium valve is prepared in metal vapors of the present invention reduction with high-purity molten-salt electrolysis titanium for raw material, adopt HDH method or atomization to prepare high-purity low-oxygen titanium valve in conjunction with metal vapors reducing process, it all innovates on raw material and purifying technique.First, on raw material is selected, choosing high-purity molten-salt electrolysis titanium is raw material, oxygen content low (being about 100ppm) in its composition, impurity content few (being about 500ppm), and does not raw materials usedly relate to high pollution production technology, environment-protecting clean.Secondly, the titanium valve obtained by hydrogenation and dehydrogenization or atomization, although oxygen content is higher, other impurity content is less, is conducive to finally obtaining high-purity low-oxygen titanium valve.By the titanium valve oxygen content low (being less than 1000ppm) that metal vapors reduction titanium valve technique finally obtains, other impurity content is extremely low (being less than 100ppm) also, and granularity is tiny, and processing performance is excellent.The industries such as the cost of this preparation method is low, efficiency is high, and the pollution caused is also little, and products obtained therefrom can be widely used in the clean processing and forming of powder metallurgy, prepared by wear-and corrosion-resistant parts, coating.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares the structural representation of the device of high-purity low-oxygen titanium valve for metal vapors reduction.
Marginal data:
1, body of heater; 2, burner hearth; 3, retort; 4, frame is expected; 5, screen cloth; 6, bell; 7, air bleeding valve; 8, Pressure gauge; 9, vacuum lead; 10, air inlet pipe; 11, hold down gag; 12, flowmeter; 13, heat-preservation cotton; 14, electrical control cubicles.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
embodiment 1:
Choosing high-purity molten-salt electrolysis titanium is raw material, adopts HDH method to the obtained titanium valve of molten-salt electrolysis titanium processing; The titanium valve that 50g hydrogenation and dehydrogenization obtains is put into vacuum seal heating furnace expects on the screen cloth of frame, selects Ca as reducing metal, and add 50gCa at vacuum seal heating furnace charge frame bottom, in extracting vacuum to vacuum seal heating furnace, vacuum reaches 8.2 × 10
-3seal after Pa, then heat up under vacuum conditions and be heated to 1278K and be incubated 2h, after having reacted, obtain high-purity titanium valve, to be cooled to room temperature, by washing high-purity titanium valve, pickling and dry remove the CaO be attached on high-purity titanium valve, obtain high-purity low-oxygen titanium valve.
embodiment 2:
Choosing high-purity molten-salt electrolysis titanium is raw material, adopts atomization to the obtained titanium valve of molten-salt electrolysis titanium processing; The titanium valve that 60g inert gas atomizer method obtains is put into vacuum seal heating furnace expects on the screen cloth of frame, selects Na as reducing metal, and add 60gNa at vacuum seal heating furnace charge frame bottom, in extracting vacuum to vacuum seal heating furnace, vacuum reaches 8.2 × 10
-3seal after Pa, then heating up under vacuum conditions is heated to 1285K and is incubated 3h, obtains high-purity titanium valve after react, to be cooled to room temperature, by washing high-purity titanium valve, the Na that is attached on high-purity titanium valve of pickling and dry removing
2o, obtains high-purity low-oxygen titanium valve.
embodiment 3:
Choosing high-purity molten-salt electrolysis titanium is raw material, adopts atomization to the obtained titanium valve of molten-salt electrolysis titanium processing; The titanium valve that rotating electrode atomized for 60g method obtains is put into vacuum seal heating furnace expects on the screen cloth of frame, selects K as reducing metal, and add 60gK at vacuum seal heating furnace charge frame bottom, in extracting vacuum to vacuum seal heating furnace, vacuum reaches 8.2 × 10
-3seal after Pa, then heating up under vacuum conditions is heated to 1273K and is incubated 2h, react and has obtained high-purity titanium valve, to be cooled to room temperature, by washing high-purity titanium valve, the K that is attached on high-purity titanium valve of pickling and dry removing
2o, obtains high-purity low-oxygen titanium valve.
embodiment 4:
Choosing high-purity molten-salt electrolysis titanium is raw material, adopts HDH method to the obtained titanium valve of molten-salt electrolysis titanium processing; The titanium valve that 55g hydrogenation and dehydrogenization obtains is put into vacuum seal heating furnace expects on the screen cloth of frame, selects Li as reducing metal, and add 55gLi at vacuum seal heating furnace charge frame bottom, in extracting vacuum to vacuum seal heating furnace, vacuum reaches 8.2 × 10
-3seal after Pa, then heating up under vacuum conditions is heated to 1288K and is incubated 2h, obtains high-purity titanium valve after react, to be cooled to room temperature, and by washing high-purity titanium valve, pickling and dry removing be attached to the Li obtained on high-purity titanium valve
2o, obtains high-purity low-oxygen titanium valve.
embodiment 5:
Choosing high-purity molten-salt electrolysis titanium is raw material, adopts atomization to the obtained titanium valve of molten-salt electrolysis titanium processing; The titanium valve that 50g PREP method obtains is put into vacuum seal heating furnace expects on the screen cloth of frame, select Mg as reducing metal, add 50gMg at vacuum seal heating furnace charge frame bottom, in extracting vacuum to vacuum seal heating furnace, vacuum reaches 8.2 × 10
-3seal after Pa, then heat up under vacuum conditions and be heated to 1275K and be incubated 2h, after having reacted, obtain high-purity titanium valve, to be cooled to room temperature, by washing high-purity titanium valve, pickling and dry remove the MgO be attached on high-purity titanium valve, high-purity low-oxygen titanium valve can be obtained.
In above-described embodiment 1 to 5, HDH method comprises hydrogenation, ball milling and dehydrogenation three steps to the processing of molten-salt electrolysis titanium, specifically, first raw material is placed in the hydrogenation of hydrogenation and dehydrogenization stove and obtains titanium hydride particles, again titanium hydride particles ball mill crushing is obtained titanium hydride powders, then titanium hydride powders is placed in hydrogenation and dehydrogenization stove Oxidative Dehydrogenation and obtains titanium valve; Atomization comprises inert gas atomizer method and rotating electrode atomized method to the processing of molten-salt electrolysis titanium, and inert gas atomizer method and rotating electrode atomized method are prior art, and wherein, namely inert gas atomizer method smashes metal liquid stream by high velocity air; Namely rotating electrode atomized method is made into pair of electrodes with metal or alloy, makes metal end face and arc contacts region become molten condition, then is thrown away by molten drop by the centrifugal force of High Rotation Speed, complete atomization process by electric discharge.
embodiment 6:
As shown in Figure 1, a kind of device preparing high-purity low-oxygen titanium valve for metal vapors reduction, comprise the body of heater 1 with furnace chamber, the middle part of furnace chamber is provided with burner hearth 2, is provided with retort 3 in burner hearth 2, material frame 4 is placed with in retort 3, material frame 4 is equiped with screen cloth 5, and leave spacing between the bottom of screen cloth 5 and retort 3, the open top end of retort 3 is sealedly connected with dismountable bell 6, bell 6 is provided with air bleeding valve 7, Pressure gauge 8 and vacuum lead 9, and retort 3 is also connected with air inlet pipe 10.
In the present embodiment, bell 6 is seal-installed on retort 3 by hold down gag 11, and in other embodiments, bell 6 also can adopt the mode such as screw, bolt to be connected with retort 3; Air inlet pipe 10 is provided with flowmeter 12.
In the present embodiment, between burner hearth 2 and body of heater 1 inwall, be filled with heat-preservation cotton 13.The outer wall of body of heater 1 is provided with electrical control cubicles 14.
In the present embodiment, body of heater 1, burner hearth 2, retort 3, material frame 4 and bell 6 are made by stainless steel.The plate of screen cloth 5 multiple circular pore for surface distributed has, this circular pore can make gas pass through and not allow titanium valve drop.Bell 6 is elevated and can be completed by electronic screw lift further, and housing by shaped steel and Plate Welding shaping, bell lining adopt fully fibrous structure, good heat insulating.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is also not only confined to above-described embodiment.For those skilled in the art, do not departing from the improvement that obtains under the technology of the present invention concept thereof and conversion also should be considered as protection scope of the present invention.
Claims (10)
1. a method for high-purity low-oxygen titanium valve is prepared in metal vapors reduction, it is characterized in that: comprise the following steps:
(1) choosing high-purity molten-salt electrolysis titanium is raw material, adopts hydrogenation and dehydrogenization or atomization to the obtained titanium valve of molten-salt electrolysis titanium processing;
(2) active metal identical for weight and titanium valve are placed in vacuum seal heating furnace, are heated to make active metal to form steam under vacuum conditions, the impurity generation reduction reaction in active metal steam and titanium valve obtains high-purity titanium valve;
(3) high-purity titanium valve is washed, pickling and the dry metal oxide removing attachment, obtain high-purity low-oxygen titanium valve.
2. method according to claim 1, is characterized in that: in described step (2), is placed in vacuum seal heating furnace to titanium valve and active metal non-direct contact.
3. method according to claim 2, is characterized in that: active metal is prepared into the bottom that particle is placed in material frame in vacuum seal heating furnace, and titanium valve is placed on the top of active metal particle by screen cloth.
4. method according to claim 1, is characterized in that: in described step (2), and heating-up temperature is 1273 ~ 1290K, and temperature retention time is 2 ~ 3 hours, and the vacuum in described vacuum seal heating furnace is 3.3 × 10
-3pa ~ 8.2 × 10
-3pa.
5. method according to claim 1, is characterized in that: described active metal is Na, K, Ca, Li or Mg.
6. method according to claim 1, is characterized in that: the addition of described active metal and titanium valve is 50 ~ 60g.
7. method according to claim 1, it is characterized in that: described HDH method comprises hydrogenation, ball milling and dehydrogenation three steps to the processing of molten-salt electrolysis titanium, specifically, first raw material is placed in the hydrogenation of hydrogenation and dehydrogenization stove and obtains titanium hydride particles, again titanium hydride particles ball mill crushing is obtained titanium hydride powders, then titanium hydride powders is placed in hydrogenation and dehydrogenization stove Oxidative Dehydrogenation and obtains titanium valve; Described atomization comprises inert gas atomizer method and rotating electrode atomized method to the processing of molten-salt electrolysis titanium.
8. prepare the device of high-purity low-oxygen titanium valve for metal vapors reduction for one kind, it is characterized in that: comprise the body of heater (1) with furnace chamber, the middle part of described furnace chamber is provided with burner hearth (2), retort (3) is provided with in described burner hearth (2), material frame (4) is placed with in described retort (3), described material frame (4) is equiped with screen cloth (5), spacing is left between the bottom of described screen cloth (5) and retort (3), the open top end of described retort (3) is sealedly connected with dismountable bell (6), described bell (6) is provided with air bleeding valve (7), Pressure gauge (8) and vacuum lead (9), described retort (3) is also connected with air inlet pipe (10).
9. device according to claim 8, is characterized in that: described bell (6) is seal-installed on retort (3) by hold down gag (11); Described air inlet pipe (10) is provided with flowmeter (12).
10. device according to claim 8, is characterized in that: be filled with heat-preservation cotton (13) between described burner hearth (2) and body of heater (1) inwall.
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| CN111558713A (en) * | 2020-06-24 | 2020-08-21 | 郑州大学 | Oxygen reduction method for small-particle-size titanium powder |
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