CN103752228B - Gas base permeation reactor - Google Patents
Gas base permeation reactor Download PDFInfo
- Publication number
- CN103752228B CN103752228B CN201410030063.1A CN201410030063A CN103752228B CN 103752228 B CN103752228 B CN 103752228B CN 201410030063 A CN201410030063 A CN 201410030063A CN 103752228 B CN103752228 B CN 103752228B
- Authority
- CN
- China
- Prior art keywords
- rare earth
- reactor
- material containing
- gas
- reducing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a gas base permeation reactor, which belongs to the technical field of metallurgy. A cool water inlet and a cool water outlet are arranged on a water cooled cover of the reactor, a reducing gas inlet pipe is arranged on the bottom of a reactor main body, one end of the reducing gas inlet pipe extends into the bottom in the reactor main body, the bottom of the reactor main body is provided with a sealing material, the sealing material is connected with the bottom of a large loading sleeve, air inlet holes are formed in the lateral wall of the lower part of the large loading sleeve along the circumference direction, and at least one small sleeve for reducing mineral powder is arranged in the large loading sleeve. The reducing gas deeply permeates and enters into the rare earth concentrate powder in gaps of a multi-layer steel net, the effective contact area of the reducing gas and the rare earth concentrate powder is improved, the reaction rate is improved, and better experiment result can be completed at lower investment in very short time, so as to reach the unforeseen experiment purpose. Moreover, the complicated preparation process of rare earth metals by the metallothermic method is avoided, and the coke which is increasingly lacked and used in the rare earth oxides agglomeration reducing method is saved.
Description
Technical field
The present invention relates to a kind of gas base permeable reactive device, belong to field of metallurgy.
Background technology
" rare earth " one word be 18th century continued to use the title of getting off because the mineral at that time for extracting this dvielement are more rare, and obtain oxide be difficult to fusing, be also difficult to water-soluble, be also difficult to be separated, it is exactly like in appearance " soil ", and is referred to as rare earth.Since 19th century, the comparative maturity of formation is that metallothermic processes (preparation of rare earth metal by metallothermic reduction) produces rare earth metal for the preparation of rare earth metal method.At high temperature with the active metallic reducing agent strong compared with rare earth, rare earth compound is reduced into the process of metal.This is the important method that rare earth metal is produced, and metallic reducing agent used has calcium, lithium, lanthanum and cerium etc.Concrete operations are dissolved in acid by the rare earth oxide being insoluble in water, obtains powder rare earth-iron-boron or sulfate through processes such as distillations, then at high temperature uses the active metallic reducing agent (calcium, lithium etc.) strong compared with rare earth that rare earth compound is reduced into metal.
Another kind of preparation method is rare earth oxide agglomeration reducing process.First richness choosing is carried out to rare earth breeze, prepare rare earth ore concentrate powder, then by powdery containing flux and the fuel of allocating right quantity in rare earths material into, Homogeneous phase mixing in mixer, to be placed on sintering machine igniting sintering, under the high temperature action produced by means of fuel combustion and a series of physical reaction effect, to produce the liquid phase of some, the solid particle other do not melted coheres into block, becomes Porous lump ore after cooling.Then lump ore is loaded in shaft furnace and allocate a certain proportion of coke into and blast high temperature wind, finally rare earth oxide is reduced into the process of metal.
But along with coke can be used day by day to reduce, price constantly rises, and gas production constantly increases, and sight is turned to the powder reduction preparation method investing gradually and more have development by people.By retrieving Patents, find that there is a lot of rare earth ore concentrate powder reduction apparatus, transverse tube type reactor is wherein favored by everybody deeply.Transverse tube type rare earth ore concentrate powder reactor great majority are made up of reative cell, barostat and sample base.Reflection room is the column type glass tube of a traverse, and respectively there is an end cap at two ends, and end cap is connected to air inlet pipe and escape pipe respectively; Inside reative cell, be placed with multiple load sample platform, multiple rare earth ore concentrate powder sample can be reduced in once experiment; Barostat is the gas current stabilization switch be connected on escape pipe, control to react room pressure by the size of by-pass cock, unsuitable too small, insufficient pressure in too small reative cell, gas and fine ore reflect that effect is bad, and breeze to be dispelled because air-flow is too fast and affects experimental result.
The concrete using method of transverse tube type rare earth ore concentrate powder reactor is placed on being taken scalar by the rare earth ore concentrate powder of testing on load sample platform, and covers both sides reative cell end cap and put into resistance-heated furnace after connecting air inlet pipe and escape pipe to fix; Energising is warming up to experimental design temperature to reative cell, then reducing gas (H2, CO, CH4 etc.) pass into from the inlet end of reaction transverse tube, gas arrives in reative cell and reacts with the rare earth ore concentrate powder surface on load sample platform, reached the object of constantly reduction by the continuous flowing of gas, the gas after reduction is discharged from outlet side; After the time reaching experimental design, stop reducing gas entering, start to pass into protective gas Ar and power-off to reative cell carry out cooling process; Just can take out sample after final reaction chamber temperature such as grade drops to room temperature and carry out precise.
But, in transverse tube type rare earth ore concentrate powder reactor, when forming fine and close metallic film on rare earth ore concentrate powder surface after gas and powdered reaction, reducibility gas is caused to be difficult to enter the inside of powder again, in order to reach required experiment effect, must the operating time be extended, increase reducing gas flow and realize.The cost that certainly will add experiment like this drops into, and more seriously reaction rate is slow, percent reduction is low, the process of impact experiment.
In sum, it is loaded down with trivial details that metallothermic processes produces rare earth metal process, and input cost is high; Reducing agent-coke-worsening shortages that rare earth oxide agglomeration reducing process uses, is unfavorable for long term growth; Although existing transverse tube type rare earth ore concentrate powder reactor meets the development of the research of rare earth ore concentrate powder reduction in the future, its reaction rate is slow, affects experiment process, needs to improve, could adapt to the fast development of world today's science and technology.
Summary of the invention
In order to overcome above deficiency, one provided by the invention can improve reaction rate rapidly, saves the reaction time, increases the percent reduction of rare earth ore concentrate powder, improves the gas base permeable reactive device of the reduction effect of gas base method.
The technical solution adopted for the present invention to solve the technical problems is:
The present invention includes: reactor water cooled cover, reactor body, reactor water black furnace covers and is provided with cooling water inlet, coolant outlet, reactor body, bottom is provided with reducing gas air inlet pipe, reactor body inner bottom part is stretched in reducing gas air inlet pipe one end, is provided with encapsulant bottom reactor body, and encapsulant is connected with the large sleeve bottom of material containing, material containing large lower cartridge sidewall circumference establishing air admission hole, being at least provided with one in the large sleeve of material containing for reducing the small sleeve of breeze.
Be micropore material carrier platform bottom described small sleeve, micropore material carrier platform is provided with lower micropore flow slowing down steel mesh, and small sleeve top is provided with micropore flow slowing down steel mesh.
Described lower micropore flow slowing down steel mesh is seven layers of setting, and described upper micropore flow slowing down steel mesh is three layers of setting.
Gas exhaust manifold on described reactor body is provided with gas base pressure maintaining valve.
The invention has the beneficial effects as follows:
Enter bottom the many reactor bodies of this reducing gas of the present invention, allow in the rare earth ore concentrate powder penetrating in multilayer steel mesh gap of reducing gas profound level, increase reducing gas and the effective contact area of rare earth ore concentrate powder, improve reaction rate, drop into lower fund in a short period of time and complete better experimental result, reach beyond thought experiment purpose.And avoid the process that metallothermic processes produces rare earth metal very complicated, save the coke of the worsening shortages that rare earth oxide agglomeration reducing process uses.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is physical form figure of the present invention.
Fig. 2 is vertical section of the present invention structural map.
Detailed description of the invention
In figure-1, cooling water inlet 1, coolant outlet 2 are welded on reactor water cooled cover 4 and are connected by washer sealing by bolt with reactor body 5, gas base pressure maintaining valve 3 is arranged on reactor body 5 the first half, the highly stable service behaviour guarantee rare earth breeze of usual needs is not blown afloat by transformation air-flow, reducing gas air inlet 6 is welded on bottom reactor body 5, reducibility gas (H
2, CO, CH
4) enter thus.
In figure-2 illustrated embodiments, all reactor parts are steel material, and gas base permeable reactive device main body 5 is cylinder, and volume is 1.9635L(diameter D is 10cm, and height H is 25cm); Reactor body 5 bottom is provided with encapsulant 15, encapsulant 15 adopts alumina powder, the large sleeve bottom of material containing is plugged in alumina powder, and material containing large lower cartridge sidewall circumference establishes air admission hole 13, is at least provided with one for reducing the small sleeve of breeze in the large sleeve of material containing.
Described material containing small sleeve 10 is arranged on the large barrel of material containing by bracket, and as shown in Figure 2, bracket surface unusual light, so obturation effect is good, prevents gas from running out of in a large number from the side, micropore material carrier platform 12 wherein in material containing small sleeve 10 is suppressed by the steel mesh of 100 meshes to form, and bearing capacity is strong, in order to avoid fine ore is scattered down, form by the steel mesh of seven layer of 60 mesh is stacked above micropore material carrier platform, small space is had between every two-layer steel mesh, feed then to respectively two material containing small sleeves 12 and (once reduce two group rare-earth breezes, be respectively charged into rare earth ore concentrate powder 70g), so rare earth ore concentrate powder is just easily filled in inside steel mesh gap, under room temperature, gas enters in reactor with 0.120m3/h, when gas enters material containing small sleeve air chamber by air admission hole, assemble in air chamber and produce faint pressure (being approximately 10-15Pa), reducing gas (H2, CO, CH4 etc.) can penetrate in rare earth powder under the effect of pressure reduction, rare earth ore concentrate powder is filled in the gap of multilayer steel mesh, reducing gas is also easy to just penetrate in the rare earth breeze in net, the climbing power of gas and the pressure of air-flow is relied on to make reducibility gas (H2 like this, CO, CH4 etc.) penetrate in rare earth powder breeze profoundly, allowing gas and breeze effectively react in such rare earth ore concentrate powder just has enough spaces to make reducibility gas permeate, micropore flow slowing down steel mesh 9 is that the steel mesh being 60 meshes by three layers of aperture is suppressed and formed, and is placed on the top of material containing small sleeve 10, plays the effect preventing powder from dispersing, the steel mesh of bottom except this effect prevent rare earth breeze in addition under the effect of leaking, to have at the bottom of sleeve storing 14 bottom material containing small sleeve 10, prevent breeze to be scattered loss, reduce experimental error.
Finally reactor body and water cooled cover 4 are added that bell seal washer 7 is connected by bolt seal; After having connected, (must from then on be carried out by mouth by the 3 pairs of reactor applications of vacuum of gas base pressure maintaining valve, otherwise immense pressure impact can make rare earth powder float) complete, then cooling water is passed into from cooling water inlet 1, energising heats up, and heating rate is set as 10 DEG C/min, waits and arrives setting experimental temperature, this contrived experiment temperature is 950 DEG C, slowly passes into reducing gas from reduction air inlet 6; Experiment to be achieved needs the time, and this contrived experiment time is 1.5h, and blowing out cools, and a gas base permeable reactive process completes.
Experiment reaction equation:
Re
xO
y+yH
2=xRe+yH
2O；
Re
xO
y+yCO=xRe+yCO
2；
Re
xO
y+y/2CH
4=xRe+y/4H
2O+y/4CO
2
Rare earth ore concentrate powder oxygen loss rate: (M
0+ 70-M
1)/70*100%
M
0---the quality of little funnel of not feeding before experiment
M
1---test the quality of little hopper of feeding
Experiment specified operational procedure is (with reducing gas H
2for example):
Weigh charging: load weighted material being loaded bottom the barrel being lined with stainless steel filtering net and to keep material tiling, barrel puts into burner hearth banking.
Vacuumize: with iron clamp, blast pipe is clamped, open vavuum pump, when Pressure gauge is-0.1MP, close vacuum pump valve and furnace roof valve, treat 3 minutes, gauge hand, as turned clockwise, illustrates gas leakage, logical argon gas is needed to hunt leak, until do not leak, if pointer still continues for air tight during-0.1MP.
Logical argon gas: open furnace roof valve, argon gas is entered from furnace roof valve by threeway, as Pressure gauge display 0MP, close furnace roof valve, open blast pipe iron clamp, argon gas is entered from furnace bottom air inlet pipe by four-way, flowmeter, adjusting gas flow (scope is at 0.08-0.1m3/h).
Program setting: empirically design of scheme experimental temperature and time (stove heating-up time per minute can not more than 10 DEG C), start to start stove temperature programming, open cooling system, water cooled cover and blast pipe.
Whether the air-tightness of inspection experimental provision: dip each tube interface place of suds brush with brush, observe and have continuously bubble to emerge, as interface has bubble to emerge, need change clamp pipe is fastening.
Logical hydrogen: reach hydrogen when starting reduction temperature, first open hydrogen valve, turn some flowmeter flows simultaneously down, after 2 points, argon gas valve cuts out, then adjust flux meter makes hydrogen flowing quantity control in the required scope of experiment (hydrogen partial pressure is less than 0.1MPa).After reduction terminates, first open argon gas valve, turn a flowmeter throughput simultaneously down, then close hydrogen valve, adjust flux meter makes argon flow amount scope at 0.08-0.1m3/h.
Blow-on samples: when stove drops to room temperature automatically, closes cooling water, and open bell and take out barrel, weigh record, sample is sealed up for safekeeping, and equipment playbacks, and whether inspection hydrogen and argon bottle close, and cuts off furnace power, terminates experiment.
Claims (2)
1. gas base permeable reactive device, it is characterized in that, comprise: reactor water cooled cover, reactor body, reactor water black furnace covers and is provided with cooling water inlet, coolant outlet, reducing gas air inlet pipe is provided with bottom reactor body, reactor body inner bottom part is stretched in reducing gas air inlet pipe one end, encapsulant is provided with bottom reactor body, encapsulant is connected with the large sleeve bottom of material containing, material containing large lower cartridge sidewall circumference establishing air admission hole, being at least provided with one in the large sleeve of material containing for reducing the material containing small sleeve of breeze; Be micropore material carrier platform bottom described material containing small sleeve, micropore material carrier platform is provided with lower micropore flow slowing down steel mesh, and material containing small sleeve top is provided with micropore flow slowing down steel mesh; The lower micropore flow slowing down steel mesh of described material containing small sleeve is seven layers of setting, and upper micropore flow slowing down steel mesh is three layers of setting, and material is all 60 mesh stainless (steel) wires.
2. gas base permeable reactive device according to claim 1, it is characterized in that, the gas exhaust manifold on reactor body is provided with gas base pressure maintaining valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410030063.1A CN103752228B (en) | 2014-01-23 | 2014-01-23 | Gas base permeation reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410030063.1A CN103752228B (en) | 2014-01-23 | 2014-01-23 | Gas base permeation reactor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103752228A CN103752228A (en) | 2014-04-30 |
| CN103752228B true CN103752228B (en) | 2015-05-13 |
Family
ID=50519636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410030063.1A Expired - Fee Related CN103752228B (en) | 2014-01-23 | 2014-01-23 | Gas base permeation reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103752228B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114733472B (en) * | 2022-04-24 | 2024-05-03 | 中国科学院长春应用化学研究所 | Reaction kettle suitable for multistage reaction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201149421Y (en) * | 2007-11-20 | 2008-11-12 | 王艳英 | Dual purpose shaft furnace reduction apparatus for coal base and gas base |
| CN102559981A (en) * | 2012-01-05 | 2012-07-11 | 中冶东方工程技术有限公司 | Iron making method and device by virtue of gas-based smelting reduction |
| CN102424876B (en) * | 2011-12-26 | 2013-07-24 | 重钢西昌矿业有限公司 | Non-blast-furnace iron making process for directly reducing vanadium titanomagnetite through gas-based shaft furnace |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01116038A (en) * | 1987-10-30 | 1989-05-09 | Nippon Mining Co Ltd | Manufacture of high purity rare earth metal |
| US6309441B1 (en) * | 1996-10-08 | 2001-10-30 | General Electric Company | Reduction-melting process to form rare earth-transition metal alloys and the alloys |
-
2014
- 2014-01-23 CN CN201410030063.1A patent/CN103752228B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201149421Y (en) * | 2007-11-20 | 2008-11-12 | 王艳英 | Dual purpose shaft furnace reduction apparatus for coal base and gas base |
| CN102424876B (en) * | 2011-12-26 | 2013-07-24 | 重钢西昌矿业有限公司 | Non-blast-furnace iron making process for directly reducing vanadium titanomagnetite through gas-based shaft furnace |
| CN102559981A (en) * | 2012-01-05 | 2012-07-11 | 中冶东方工程技术有限公司 | Iron making method and device by virtue of gas-based smelting reduction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103752228A (en) | 2014-04-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mousa et al. | Effect of nut coke-sinter mixture on the blast furnace performance | |
| CN108149016A (en) | Manganese-silicon integrated smelting system | |
| CN115666890A (en) | Method and system for treating concrete particles | |
| CN103752228B (en) | Gas base permeation reactor | |
| CN103966402B (en) | RH vacuum refining system and sulfur method for molten steel desulfurizing | |
| CN206570363U (en) | CO in VOD furnace exhaust gas2, CO Ar circulation injection steel-smelting device | |
| CN209210535U (en) | A kind of PCB etching waste liquor processing unit | |
| CN107195339A (en) | A kind of fluent metal loop operation melting media and purifier | |
| CN102294170B (en) | Titanium high temperature electrolytic furnace special-purpose tail gas processing system | |
| CN102433170A (en) | Preparation method for ferrum-silicon complex desulfurizer | |
| CN206290693U (en) | A kind of new pressure vessel | |
| CN104152684B (en) | A kind of cylinder Horizontal normal pressure strengthening leaching tanks | |
| CN214862419U (en) | Blowing gas ammonia desulfurization system | |
| CN201862367U (en) | Dissolving tank | |
| CN207964444U (en) | A kind of iron ore loads with lotus low temperature reduction degradation test device | |
| CN204247173U (en) | The solid-liquid reaction gas generating unit that a kind of gas speed is adjustable | |
| CN207085670U (en) | A kind of bend pipe container type air filter | |
| CN207605714U (en) | A kind of multi-stage fixed-bed reaction unit for producing 2,2`- bipyridyls | |
| CN206116532U (en) | Mixing arrangement of battery solution solvent | |
| CN106636559B (en) | The steel-smelting device of CO2, CO-Ar cycle injection in VOD furnace exhaust gas | |
| CN204973291U (en) | Amine liquid filters defoaming composite treatment device | |
| CN205473923U (en) | Membrane bioreactor combines ion exchange's ore device that soaks | |
| CN203954995U (en) | Sintering flue gas desulfurization system and desulfurizing agent adding set thereof | |
| CN109628676A (en) | A kind of abbreviated system directly producing pure molten iron | |
| CN111394730B (en) | Etching solution regeneration device and etching solution regeneration method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150513 Termination date: 20180123 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |