CN1726294A - Method and device for carrying out a tribochemical reaction - Google Patents
Method and device for carrying out a tribochemical reaction Download PDFInfo
- Publication number
- CN1726294A CN1726294A CNA2003801061623A CN200380106162A CN1726294A CN 1726294 A CN1726294 A CN 1726294A CN A2003801061623 A CNA2003801061623 A CN A2003801061623A CN 200380106162 A CN200380106162 A CN 200380106162A CN 1726294 A CN1726294 A CN 1726294A
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- China
- Prior art keywords
- reaction
- titanium
- medium
- metal
- spherolite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1204—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
- C22B34/1209—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
- C22B34/1222—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes using a halogen containing agent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1281—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using carbon containing agents, e.g. C, CO, carbides
Abstract
The invention relates to a method and device for carrying out a tribochemical reaction, during which Faraday instabilities are produced by the spatial to-and-fro movement of a medium that is granular, grainy or made of balls. Tribochemical reaction conditions are produced with the aid of Faraday instabilities at points of contact of particles of the medium. The medium can either participate in the reaction or behave inertly with regard to the other educts. The method is suited for extracting (raw) titanium and titanium oxide from titaniferous minerals, for example, ilmenite and rutile.
Description
The invention belongs to the friction chemical reaction field, and be particularly related to a kind of use of the faraday's unstable (Faraday-Instabilitaten) when carrying out friction chemical reaction.
Background technology
Now known, can be according to the Kroll method at rotary oven or in fluid bed furnace and under about 800-1000 ℃, utilize carbon and chlorine and from known titaniferous ore, as making titanium tetrachloride in ilmenite or the rutile.Then, behind corresponding purification process (crystallization is also then being distilled under 136 ℃), under about 800-1000 ℃, the titanium tetrachloride of liquid state is reduced into the titanium cavernous body with liquid magnesium.Wash the magnesium chloride that forms in this process and again electrolytic reduction become magnesium, and it is sent back in the production process again.
The titanium cavernous body and is combined with a large amount of oxygen because its surface-area is bigger, these oxygen in the expection metal that will produce not as alloy compositions.The titanium cavernous body must be carried out fragmentation, and pulverize, be pressed into electrode, in electric arc, utilize zone melting process then and be fused into fine and close metal titanium.All method stepss that relate to titanium all will carry out under protective atmosphere (rare gas), to avoid oxidation.
In order to make pure especially titanium, the titanium tetra iodide that is obtained from titanium tetrachloride will be decomposed on 1300 ℃ of red-hot tungsten filaments.
Detailed Description Of The Invention
Task of the present invention is to provide a kind of friction chemical reaction that is used to implement, and can avoid better method of the prior art, the particularly defective in the titanium production process and better device.
In addition, task of the present invention also is, produce a kind of special friction chemical reaction situation by means of the faraday's unstable that in particle (the preferred particulates diameter is 0.1 to 20mm particle) medium, produces, and this situation can be utilized friction chemical reaction and isolating mixture is directly changed into product.Wherein, described granule medium can be according to the difference of the reaction that will carry out, or participates in reaction, or is inertia with respect to reaction product and educt.
In addition, task of the present invention also is, produce a kind of special friction chemical reaction situation by means of the faraday's unstable that in particle (the preferred particulates diameter is 0.1 to 20mm the particle) medium of ore in sand form/ore, produces, this situation can be utilized reductive agent and halogen gas and the oxidizing reaction by heterogeneous catalytic reaction and reductive agent, and ore in sand form/ore particles is directly changed.
Relevant with the production of titanium, task of the present invention also particularly in, make a kind of special friction chemical reaction situation by means of faraday's unstable that the granule medium (the preferred particulates diameter is 0.1 to 20mm particle) at ore in sand form/ore (for example ilmenite or rutile) produces, this situation can be by means of reductive agent, preferably carbon monoxide and halogen gas (preferred iodine or chlorine) are by the oxidizing reaction of heterogeneous catalytic reaction and reductive agent, for example carbon monoxide is oxidized to the oxidizing reaction of carbonic acid gas, and the ore in sand form/ore particles that preferably only contain conventional associated element directly is converted to metal titanium.
Relevant with the production of titanium dioxide, task of the present invention also is, make a kind of special friction chemical reaction situation by means of faraday's unstable that the granule medium (the preferred particulates diameter is 0.1 to 20mm particle) at ore in sand form/ore (for example ilmenite or rutile) produces, this situation can be by reductive agent, preferably carbon monoxide and halogen gas (preferred chlorine) and the oxidizing reaction by heterogeneous catalytic reaction and reductive agent, for example carbon monoxide is oxidized to the oxidizing reaction of carbonic acid gas, and ore in sand form/ore particles is directly changed into titanium dioxide.
Task of the present invention can be solved by content described in the independent claim.
The present invention has comprised following thought, promptly in the process of carrying out friction chemical reaction, in granule medium or the medium be made up of spherolite, by last/motion and obtain faraday's unstable down.Granule medium moves up and down in gravity field, thereby reaches a kind of special state, and promptly the particle windrow has the behavioral trait that is similar to the liquid phase that is made of solid ingredient under this state.In this state, faraday's unstable appears on the particulate of granule medium.Faraday's unstable is by particulate state, microgranular or produced by the moving up and down of medium that spherolite constitutes, simultaneously, utilize this faraday's unstable that on the point of contact/contact position of media components, occurs, just can form the friction chemical reaction condition of carrying out friction chemical reaction.Than traditional method (rotary oven or fluid bed furnace), faraday's unstable that utilization occurs in the medium of particulate state or spherolite formation is carried out this scheme of friction chemical reaction and is had following advantage, i.e. reaction can be carried out in a more favourable thermokinetics scope.
In granule medium, faraday's unstable causes generating a kind of form with some mechanical energy higher zone (Muster) relevant with volume or volume time.In these zones, under relatively low temperature, just can carry out friction chemical reaction between granular or the globular particle or between granular or particle that globular collides mutually.
In contrast to known fluidized bed process, the advantage of utilizing faraday's unstable to carry out friction chemical reaction is, granular and utilize in the unsettled fluidized-bed of faraday and can form excitation area, in these zones, in than traditional fluidized-bed, just can carry out friction chemical reaction under the lower temperature.
In the process that is used for preparing metal, the advantage of this method is, by with the heterogeneous catalyst between more efficiently mineral, reductive agent (for example carbon monoxide) and the halogen gas gas-solid-reaction uses the reduction reaction of the metal oxide (mineral) that carbon and halogen gas carry out, and generate metal halide and carbonic acid gas and substitute.
Be equipped with according to the titanium tetra iodide legal system titanium aspect, the advantage of this method is, no longer need the sort of high energy consumption and the rapid preparation process of multistep that must make titanium by the very high titanium cavernous body of technical costs from titanium ore by use, the substitute is not needs via this intermediate steps of titanium cavernous body, energy-conservation and the preparation process of a step only arranged.
Be equipped with according to the titanium tetrachloride legal system aspect the titanium white (titanium dioxide), the advantage of this method is, can replace multistep process with a kind of a one-step process (adding oxygen in the titanium tetrachloride streams).
Embodiment
Below will and come more at large to set forth the present invention in conjunction with the accompanying drawings according to embodiment.Here accompanying drawing is:
Fig. 1 is the device synoptic diagram that is used to implement friction chemical reaction, has wherein utilized faraday's unstable; With
Fig. 2 has wherein utilized faraday's unstable for another device synoptic diagram that is used to implement friction chemical reaction.
What Fig. 1 showed is the device 1 that a kind of faraday's of utilization unstability is implemented friction chemical reaction. Device 1 is particularly suitable for preparing thick titanium (titanium tetrahalide), and is further used for adding from the ore in sand form/ore of titaniferous The worker becomes titanium or titanium white (titanium dioxide).
For implementing the method, need to spread ore in sand form or ore at the plate of level or the dish 9 of level. By Make plate/dish 9 along movement in vertical direction in a mobile device 5. As mobile device 5 can be especially excellent Choosing is pneumatic motor, hydraulic cylinder or straight line magnetic field driver. Motion mode with vertical direction is to make at grain Produce faraday's unstability in shape ore in sand form or the ore. This motion process can be especially preferably with periodic or Mixed and disorderly formula is carried out.
Utilize input unit 7 just can the educt fluid be imported in the reaction mixture by the hole.If will obtain the situation of titanium or titanium dioxide, then refer to gaseous halide and carbon monoxide here as reductive agent.The reaction compartment and the external environment of device 1 separate.Special preferably sidewall by reactor bottom 8 of this isolation and outer cover 3 realize that wherein said sidewall is preferably designed to right cylinder, outer cover then in division surface 4 sidewall with respect to reactor bottom 8 seal.For example, can in division surface 4, load onto simultaneously the sealing member (not shown) in that flange is set on the outer cover 3.For protecting gas to charge in the reaction compartment, at least one inlet 6 will be set.And this inlet can be preferably mounted on the reactor lower part 8.
In order from reaction compartment, to discharge gaseous reaction products, at least one opening 2 will be set, and they are preferably mounted on the outer cover 3 of reactor on reaction compartment.As substituting or additional project of opening 2, can be particularly preferably in some heatable plain conductors be installed on the outer cover of reactor, and titanium tetrahalide with regard to precipitable on these metal wires and decompose.If the iodide of titanium then can be, for example tungsten filament here.
Another opening (not shown) also can be set import to reaction compartment in order to the oxygen that will be used for preparing titanium dioxide from titanium tetrachloride.Yet this import operation also can at first---discharged titanium tetrachloride the back---from reaction compartment carry out, reaction product is by opening 2 after this.
What Fig. 2 showed is a kind of device 20 of the Fig. 1 of being similar to device, and it is used to utilize faraday's unstable to implement friction chemical reaction.Technical characterictic identical among the figure is represented with identical mark.Device 20 among Fig. 2 is that with the difference of the device of Fig. 1 running gear 5 is set at outside the reaction chamber of device 20.The advantage of doing like this is that reaction educt, intermediate product and finished product can not corrode or damage running gear.In this case, higher load capacity has been considered in this topology layout of running gear 5.
Will the ore in sand form/ore through grinding be placed on one in gravity field on the dish with the vertical direction up-down vibration, and make it be in a kind of special state, the particle windrow has the behavioral trait that is similar to the liquid phase that is made of solid ingredient under this state.In this process, on the interface between liquid particles layer and (protection) gas phase, constitute faraday's unstable, for example with the form of the oscillogram of spatial stability.Here, preferably use rare gas element, be more preferably rare gas, preferably argon and helium as protection gas.If each particle collides mutually in the special lasing region of this layer, then be positioned at gas mutual catalysis generation friction chemical reaction on position of collision of reaction compartment subsequently.For example, if handle the ore of titanium ore, titanium, then just try hard to obtain titanium/titanium oxide as end product.
The product of this reaction at first is a kind of metal-salt or metal complex.The product that this reaction of titanium ore/titanium ore is arranged then is a kind of titanium tetrahalide, and it can distil or flash to gas.
If requirement is arranged,, then under comparatively high temps, in sublimate, mix a certain amount of oxygen, and be oxidized to titanium dioxide as under the situation of titanium tetrachloride, directly therefrom making titanium dioxide.Wherein the chlorine of Xing Chenging can turn back in the process again.
If require directly therefrom to make metal titanium under the situation of titanium tetra iodide, then sublimate/steam is for example resolving into fine and close titanium and iodine under about 1300 ℃ on the electrically heated tungsten filament.Iodine can send back in the process more again and goes.
Described method and the device 1 and 20 of being set forth can be used for carbon-free preparation metal and metal oxide from metallic ore.In heterogeneous gas-solid reaction, utilize reductive agent and a kind of halogen can make metal-salt or complex compound.Further process this metal-salt/complex compound then.The solution of multiple metal-salt can be by means of separating as the method that is documented among International Patent Application PCT/DE02/01377.
For example, aforesaid those methods also applicable to from known titaniferous ore, for example make (slightly) titanium and titanium dioxide in ilmenite and the rutile.Be preferably in utilization and form corresponding titanium halide in the heterogeneous gas-solid reaction of carbon monoxide reducing agent and a kind of halogen.Except using carbon monoxide, also preferably use chlorine or iodine as the halogen in the gas-solid reaction, thereby form titanium tetrachloride or titanium tetra iodide.With known traditional method, titanium tetrachloride is processed into the titanium of titanium cavernous body form with magnesium then.But titanium tetra iodide then can distil and produce pure titanium under thermolysis, need not form cavernous body simultaneously.
Disclosed feature of the present invention can independent and any combination in aforementioned specification, claims and accompanying drawing, implements the present invention with various embodiments.
Claims (9)
1. in order to implement the method for friction chemical reaction, it is characterized in that, by granular, spherical or carry out moving back and forth in the space by the medium that spherolite constitutes and produce faraday's unstable, and form the friction chemical reaction condition by means of the faraday's unstable on the contact position/point of contact of media particle.
2. the method for claim 1 is characterized in that, uses and not to participate in the molding that reacts, and special preferably spherolite is as the medium of implementing reaction.
3. method as claimed in claim 1 or 2 is characterized in that, uses the inert metal spherolite, especially preferably the refining steel spherolite.
4. the method for claim 1 is characterized in that, uses and self participates in the medium of reaction, and especially preferably ore in sand form is implemented reaction as medium.
5. as the purposes of method as described in one of claim 1 to 4, it is used for carbon-free preparation metal and metal oxide.
6. as the purposes of method as described in one of claim 1 to 4, it is used for carbon-free preparation titanium and titanium dioxide.
7. as the purposes of method as described in one of claim 1 to 4, it is used for carbon-free preparation metal complex.
8. as the purposes of one of claim 1 or 4 described method, it is used for carbon-free preparation metal and metal oxide, and wherein each composition of the material that will be made by ore separates, therefrom to make metal, metal-salt or metal oxide.
9. in order to implement device as the described method of one of claim 1 to 4, it has the reaction compartment of a sealing, wherein design has a carrier side that is used to carry medium granular, spherical or that be made of spherolite, described carrier side is connected on the running gear simultaneously, utilize this device, granular, spherical or can move back and forth by the medium that spherolite constitutes, thus be used for producing faraday's unstable on the media particle of friction chemical reaction.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10249163.1 | 2002-10-22 | ||
| DE10249163A DE10249163A1 (en) | 2002-10-22 | 2002-10-22 | Method and device for using Faraday instabilities to carry out tribochemical reactions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1726294A true CN1726294A (en) | 2006-01-25 |
| CN100493784C CN100493784C (en) | 2009-06-03 |
Family
ID=32087096
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003801061623A Expired - Fee Related CN100493784C (en) | 2002-10-22 | 2003-10-22 | Method and device for carrying out a friction chemical reaction |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP1558774B1 (en) |
| CN (1) | CN100493784C (en) |
| AT (1) | ATE385523T1 (en) |
| AU (1) | AU2003281966A1 (en) |
| DE (2) | DE10249163A1 (en) |
| WO (1) | WO2004038048A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8329626B2 (en) * | 2010-06-24 | 2012-12-11 | Johnson & Johnson Consumer Companies, Inc. | Low-irritating, clear cleansing compositions with relatively low pH |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NZ273552A (en) * | 1993-09-13 | 1996-12-20 | Univ Australian | Treatment of titaniferous ore by high energy milling in the presence of an additive; leaching iron from milled product |
| JP2885098B2 (en) * | 1994-10-07 | 1999-04-19 | 株式会社栗本鐵工所 | Processing method of titanium sponge powder |
| ATE185995T1 (en) * | 1995-05-26 | 1999-11-15 | Goldschmidt Ag Th | METHOD FOR PRODUCING X-RAY MOPHER AND NANOCRYSTALLINE METAL POWDER |
| AU2002312720A1 (en) * | 2001-04-12 | 2002-10-28 | Mir-Chem Gmbh | Method and device for extracting and separating substances |
-
2002
- 2002-10-22 DE DE10249163A patent/DE10249163A1/en not_active Withdrawn
-
2003
- 2003-10-22 WO PCT/DE2003/003525 patent/WO2004038048A1/en active IP Right Grant
- 2003-10-22 DE DE50309132T patent/DE50309132D1/en not_active Expired - Fee Related
- 2003-10-22 AT AT03773570T patent/ATE385523T1/en not_active IP Right Cessation
- 2003-10-22 AU AU2003281966A patent/AU2003281966A1/en not_active Abandoned
- 2003-10-22 EP EP03773570A patent/EP1558774B1/en not_active Expired - Lifetime
- 2003-10-22 CN CNB2003801061623A patent/CN100493784C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| WO2004038048A1 (en) | 2004-05-06 |
| CN100493784C (en) | 2009-06-03 |
| EP1558774A1 (en) | 2005-08-03 |
| AU2003281966A1 (en) | 2004-05-13 |
| DE10249163A1 (en) | 2004-05-06 |
| DE50309132D1 (en) | 2008-03-20 |
| ATE385523T1 (en) | 2008-02-15 |
| EP1558774B1 (en) | 2008-02-06 |
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Granted publication date: 20090603 Termination date: 20091123 |