CN109848430A - Process for preparing metallic titanium by using titanium dioxide - Google Patents
Process for preparing metallic titanium by using titanium dioxide Download PDFInfo
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- CN109848430A CN109848430A CN201811538474.6A CN201811538474A CN109848430A CN 109848430 A CN109848430 A CN 109848430A CN 201811538474 A CN201811538474 A CN 201811538474A CN 109848430 A CN109848430 A CN 109848430A
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- Prior art keywords
- titanium
- powder
- furnace body
- titanium dioxide
- technique
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000010936 titanium Substances 0.000 title claims abstract description 41
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 39
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 47
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 22
- 238000003825 pressing Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 238000007731 hot pressing Methods 0.000 claims abstract description 7
- 239000000376 reactant Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 5
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002485 combustion reaction Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 238000005984 hydrogenation reaction Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000001569 carbon dioxide Substances 0.000 abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 abstract description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000292 calcium oxide Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 11
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 241000790917 Dioxys <bee> Species 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to the preparation of metallic titanium, in particular to a process for preparing metallic titanium by utilizing titanium dioxide, which comprises the steps of introducing calcium carbonate powder and titanium dioxide powder into a furnace body and uniformly mixing; pressing and sintering the mixed powder in a furnace body, and collecting gas; pushing the pressed and sintered reactant out of the furnace body, adding calcium hydride powder, mixing uniformly, and placing in a vacuum furnace for hot-pressing reduction; acid washing and filtering the product of the hot-pressing reduction to obtain a filtered substance; washing the filtered material with water, and drying to obtain the metal titanium. The invention adopts calcium carbonate and carbon dioxide as raw materials, realizes the process for preparing the metal titanium from the titanium dioxide by the working procedures of mixing, pressing, sintering, crushing, mixing, vacuum reduction and the like, and can generate the calcium carbonate by utilizing the reaction of gas generated in the sintering and the final product calcium oxide, thereby realizing the recycling of the product, saving the raw materials and reducing the cost.
Description
Technical field
The present invention relates to the preparation of Titanium, specifically a kind of technique for preparing Titanium using titanium dioxide.
Background technique
Titanium valve belongs to bulk material, the performance synthesis general character of Titanium base and body of powder.It is numerous excellent due to titanium valve
Property, be widely used in aerospace, chemical industry, petroleum, metallurgy and ship, high performance titanium or titanium alloy biomaterial,
The fields such as energy and material, electronic material.The key industry production method of titanium valve at present, with Titanium (such as titanium sponge, titanium ingot, titanium
Bits, residual titanium etc.) be raw material, in hydrogenation furnace under positive hydrogen pressure 700~900 DEG C make its saturation inhale hydrogen, brittle hydrogen can be formed
Change titanium, then titantium hydride is milled into powder, finally obtains pure titanium valve in 500 DEG C or so progress dehydrogenations.This method has production
Powder size range is wide, process is easily achieved, it has also become the main method of titanium valve is produced both at home and abroad, but when application this method, it is former
Material consuming is more, be easy to cause waste, and equipment is more, structure is complicated, causes cost of investment high, production efficiency.
Summary of the invention
In view of the above technical problems, the present invention a kind of energy saving is provided, improve production efficiency utilize titanium dioxide system
The technique of standby Titanium.
The technical scheme of the invention to solve the technical problem is: a kind of prepare Titanium using titanium dioxide
Technique comprising following steps:
(1) calcium carbonate powder and titania powder furnace body is imported to be uniformly mixed；
(2) the above-mentioned mixed-powder of compacting sintering in furnace body, and collect gas；
(3) reactant after compacting sintering is released into furnace body, and hydrogenation calcium powder is added and is uniformly mixed, then is placed in vacuum drying oven hot
Pressure reduction；
(4) product of pickling filtering hot pressing reduction, obtains filtering object；
(5) upper object is filtered in washing, and is dried, and Titanium is obtained.
Preferably, the filtrate of pickling and washing is collected, and the gas for importing into the filtrate above-mentioned collection is reacted,
Precipitating is generated, then crushes, dry sediment, calcium carbonate powder is obtained, calcium carbonate powder is then recycled to the furnace body.
Preferably, the upper of furnace body is equipped with mixing chamber, lower part is equipped with the combustion chamber communicated with the mixing chamber, it is described mixed
It closes room two sides and is equipped with feed inlet, furnace body top is equipped with exhaust outlet, titania powder and calcium carbonate powder and is distinguished by air-flow
It is delivered to mixing chamber from the feed inlet of furnace body two sides to be mixed, air-flow is flowed out from the exhaust outlet after powder mixing, mixing
Powder is sintered into the combustion chamber under the effect of gravity.
Preferably, being equipped with pressing plate moving up and down in the mixing chamber, which is moved to combustion chamber to mixing
Powder is suppressed.
Preferably, being provided with the worm screw that can protrude into the mixing chamber on the furnace body, it is equipped with and the worm screw at the top of furnace body
The inserting end of the worm gear of cooperation, the worm screw connects the pressing plate.
Preferably, be provided in the axial direction with air flue in the worm screw, offered on the pressing plate be connected to the air flue it is logical
Hole, the gas that compacting sintering generates are collected after through-hole and air flue outflow.
Preferably, the reactant after moving down the compacting sintering of release by pressing plate is uniformly mixed with calcium hydride after crushing,
It is delivered to vacuum drying oven again.
Preferably, the temperature of compacting sintering is 450-550 DEG C.
Preferably, the temperature of vacuum hotpressing is 500-600 DEG C.
As can be known from the above technical solutions, the present invention uses calcium carbonate and carbon dioxide for raw material, passes through mixing, compacting, burning
The processes such as knot, broken mixing, vacuum reduction realize the technique that Titanium is prepared from titanium dioxide, using producing in sintering
Raw gas reacts generation calcium carbonate with final product calcium oxide and has saved raw material to realize recycling for product, drops
Low cost.
Specific embodiment
The present invention is described in detail below, illustrative examples of the invention and explanation are used to explain the present invention herein, but
It is not as a limitation of the invention.
The present invention provides a kind of techniques for preparing Titanium using titanium dioxide comprising following steps:
It is uniformly mixed firstly, calcium carbonate powder and titania powder are imported furnace body；The above-mentioned mixing of compacting sintering in furnace body
Powder, and collect gas, i.e. carbon dioxide gas；The present invention uses closed furnace body, which is equipped with mixing chamber, lower part
Equipped with the combustion chamber communicated with the mixing chamber, the mixing chamber two sides are equipped with feed inlet, and furnace body top is equipped with exhaust outlet, dioxy
Change titanium powder and calcium carbonate powder is delivered to mixing chamber from the feed inlet of furnace body two sides respectively by air-flow and is mixed, powder is mixed
Air-flow is flowed out from the exhaust outlet after conjunction, and mixed powder is sintered into the combustion chamber under the effect of gravity.Implementing
In the process, powder is conducive to dispersion powders by air-flow conveying, guarantees titania powder and calcium carbonate powder in mixing chamber
It is uniformly mixed.
Preferably, the feed inlet of the furnace body two sides is arranged along furnace body tangential direction, so that powder is in airflow function
Under in mixing chamber formed vortex, further realize dispersion；One of feed inlet is arranged on the upside of mixing chamber, another charging
Mouth is arranged on the downside of mixing chamber, and the vortex that the two generates instead gives birth to collisional mixing in mixing chamber, so that powder mixing is more uniform.It is mixed
Taper big in upper end, that lower end is small can be designed by closing room bottom, and the small cone mouth in lower end connects the combustion chamber.Powder after anti-raw collision
End is collected to cone mouth under the effect of gravity, thus flowing in combustion chamber.Combustion chamber can be cylindrical, and the diameter of cylinder and lower end are small
Cone mouth diameter is equal.On the one hand combustion chamber compared to the small-diameter circular column of furnace body is conducive to arrange heat source, saving in furnace body
On the other hand space is conducive to collect, suppresses mixed-powder.
Be equipped with pressing plate moving up and down in mixing chamber of the invention, the pressing plate be moved to combustion chamber to mixed powder into
Row compacting.Again using 450-550 DEG C of sintering after mixed-powder is repressed, be conducive to generate calcium titanate.Specifically, the furnace body
On be provided with the worm screw that can protrude into the mixing chamber, the worm gear cooperated with the worm screw is equipped at the top of furnace body, the worm screw protrudes into
End connects the pressing plate.Worm gear is rotated in implementation process to drive worm screw to move up and down, so that pressing plate is driven to move up and down, it is real
Now to the compacting of mixed-powder.And the diameter of pressing plate is preferably equal or smaller with the diameter of combustion chamber, if the diameter of pressing plate is too
Small, it is uniform that it will cause underpressings.Simultaneously because using cylindrical combustion chamber, powder itself can sink under the effect of gravity
Drop, therefore lesser press power can be used.Thus the present invention realizes the compacting of powder using worm and gear, not only structure letter
Single, operation is easy, and cost is relatively low.
It is provided in the axial direction with air flue in the worm screw, the through-hole being connected to the air flue is offered on the pressing plate, in dioxy
Change in titanium powder and calcium carbonate powder reaction process, pressing plate suppresses always mixed-powder, on the one hand guarantees that reaction is constantly in
Under pressure state, be conducive to the progress of reaction；On the other hand advantageous exhaust, because of titania powder and calcium carbonate powder reaction
Carbon dioxide gas can be generated in the process, and generating carbon dioxide gas at this time then can be from the through-hole of pressing plate and the upper airway flow of worm screw
Out, not only easy to exhaust, but also convenient for collecting gas.Bottom is equipped with discharge port in burning, and is covered with bottom plate on discharge port, can
The compacting to mixed-powder is realized with pressing plate, bottom plate is flexibly connected with furnace body, and the powder sintered of compacting is in bulk after the reaction was completed,
As long as opening bottom plate when discharging, is moved down by pressing plate and release blocky reactant from discharge port, collection material is significantly facilitated, into one
Step improves production efficiency.
From the foregoing, it will be observed that the present invention realizes calcium carbonate powder and carbon dioxide in such a way that mixing chamber and combustion chamber combine
The process of mixing, compacting and the sintering of powder raw material, with existing independent use mixing apparatus, press device and sintering furnace phase
Than, not only high production efficiency, at low cost, and device structure is simple, easily operated.
It after reactant after compacting sintering releases furnace body, is crushed, adds hydrogenation calcium powder and be uniformly mixed, then set
In using 500-600 DEG C of hot pressing reduction in vacuum drying oven, at this point, calcium hydride resolves into calcium, the calcium titanate with compacting sintering production
Reaction generates Titanium and calcium oxide, is achieved in the preparation by titanium.Then pickling filtering is carried out to Titanium and calcium oxide, i.e.,
Object is titanium in filter, then washes Titanium, and dry, and obtains Titanium.Preferably, collecting the filtrate of pickling and washing, at this time
Due to containing water in filtrate, calcium oxide can hydrolyze hydrate, in the carbon dioxide for importing above-mentioned collection into the filtrate, i.e.,
Precipitation of calcium carbonate is generated, then crushes, dry sediment, calcium carbonate powder is obtained, calcium carbonate powder is then recycled to the furnace
Body, it is thus achieved that the recycling of gas, and raw material is generated with final product, thus not only gas is realized back
It receives, and obtains raw material, production cost is greatly saved.
Above embodiment is used for illustrative purposes only, and is not limitation of the present invention, related technical field
Those of ordinary skill without departing from the spirit and scope of the present invention can be with various changes can be made and modification, therefore institute
There is equivalent technical solution also to should belong to scope of the invention.
Claims (9)
1. a kind of technique for preparing Titanium using titanium dioxide, feature the following steps are included:
(1) calcium carbonate powder and titania powder furnace body is imported to be uniformly mixed；
(2) the above-mentioned mixed-powder of compacting sintering in furnace body, and collect gas；
(3) reactant after compacting sintering is released into furnace body, and hydrogenation calcium powder is added and is uniformly mixed, then is placed in vacuum drying oven hot
Pressure reduction；
(4) product of pickling filtering hot pressing reduction, obtains filtering object；
(5) upper object is filtered in washing, and is dried, and Titanium is obtained.
2. the technique for preparing Titanium using titanium dioxide according to claim 1, it is characterised in that: collect pickling and washing
Filtrate, and the gas for importing into the filtrate above-mentioned collection is reacted, and generates precipitating, then crush, dry sediment, acquisition
Then calcium carbonate powder is recycled to the furnace body by calcium carbonate powder.
3. the technique according to claim 1 or claim 2 for preparing Titanium using titanium dioxide, it is characterised in that: on the furnace body
Portion is equipped with mixing chamber, lower part is equipped with the combustion chamber communicated with the mixing chamber, and the mixing chamber two sides are equipped with feed inlet, furnace body top
End is equipped with exhaust outlet, titania powder and calcium carbonate powder and is delivered to mixing from the feed inlet of furnace body two sides respectively by air-flow
Room is mixed, and air-flow is flowed out from the exhaust outlet after powder mixing, and mixed powder enters the burning under the effect of gravity
Room is sintered.
4. the technique for preparing Titanium using titanium dioxide according to claim 3, it is characterised in that: set in the mixing chamber
There is pressing plate moving up and down, which is moved to combustion chamber and suppresses mixed powder.
5. the technique for preparing Titanium using titanium dioxide according to claim 4, it is characterised in that: be arranged on the furnace body
There is the worm screw that can protrude into the mixing chamber, the worm gear cooperated with the worm screw, the inserting end connection of the worm screw are equipped at the top of furnace body
The pressing plate.
6. the technique for preparing Titanium using titanium dioxide according to claim 5, it is characterised in that: along axis in the worm screw
To air flue is offered, the through-hole being connected to the air flue is offered on the pressing plate, the gas that compacting sintering generates is gentle along through-hole
It is collected after road outflow.
7. the technique for preparing Titanium using titanium dioxide according to claim 6, it is characterised in that: move down release by pressing plate
Compacting sintering after reactant be uniformly mixed after crushing with calcium hydride, then be delivered to vacuum drying oven.
8. the technique for preparing Titanium using titanium dioxide according to claim 1, it is characterised in that: the temperature of compacting sintering
It is 450-550 DEG C.
9. the technique for preparing Titanium using titanium dioxide according to claim 1, it is characterised in that: the temperature of vacuum hotpressing
It is 500-600 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811538474.6A CN109848430A (en) | 2018-12-18 | 2018-12-18 | Process for preparing metallic titanium by using titanium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811538474.6A CN109848430A (en) | 2018-12-18 | 2018-12-18 | Process for preparing metallic titanium by using titanium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109848430A true CN109848430A (en) | 2019-06-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811538474.6A Withdrawn CN109848430A (en) | 2018-12-18 | 2018-12-18 | Process for preparing metallic titanium by using titanium dioxide |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705720A (en) * | 2020-12-24 | 2021-04-27 | 中国科学院过程工程研究所 | Preparation method of low-oxygen titanium powder |
-
2018
- 2018-12-18 CN CN201811538474.6A patent/CN109848430A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705720A (en) * | 2020-12-24 | 2021-04-27 | 中国科学院过程工程研究所 | Preparation method of low-oxygen titanium powder |
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Application publication date: 20190607 |