CN1039593C - Calcining system and technique for fluidized bed-mobile bed mixed reactor - Google Patents
Calcining system and technique for fluidized bed-mobile bed mixed reactor Download PDFInfo
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- CN1039593C CN1039593C CN94116925A CN94116925A CN1039593C CN 1039593 C CN1039593 C CN 1039593C CN 94116925 A CN94116925 A CN 94116925A CN 94116925 A CN94116925 A CN 94116925A CN 1039593 C CN1039593 C CN 1039593C
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Abstract
The present invention relates to a quasi multi-layer mixed type calcining device of fluidized beds and moving beds. A cylindrical air distribution column is arranged in a cylindrical reaction pipe to form multiple layers of spiral ascending air flow; reaction is carried out in an annular quasi multi-layer fluidized bed in a temperature distribution field having a low-temperature region, a medium-temperature region and a high-temperature region from top to bottom; particulate material containing 8% of adsorbed water is continuously and quantitatively added in the annular quasi multi-layer fluidized bed to be dewatered, oxidized and decomposed to enter a medium-temperature moving bed under the annular quasi multi-layer fluidized bed; the material is quantitatively discharged from a closed discharge device after cooled by a cooling section; the system is greater than or equal to 99%, the electricity consumption is 3 kwh/h, the ignition loss is less than or equal to 0.5%, and the yield is 10 kg/h.
Description
The present invention is a kind of high-temperature fluidizedization bed-moving-bed mixed type gas solid reactor, belong to granular material oxidizing roasting or roasting prepares the micro mist material in inert atmosphere technical field, wherein preferentially belong to the technical field of producing rare earth oxide by rare earth oxalate or carbonated rare earth.
Roasting becomes the technical requirements of rare earth oxide very high to rare-earth industry to rare earth oxalate: require the efficient of roasting reactor very high, reactivity 〉=99%; The rate of recovery of requirement system 〉=99%; Requirement is reduced to the contamination degree minimum.Up to the present rare-earth industry is mainly taked fixed bed type reactor one crucible method for this reason, comprising cabinet-type electric furnace and tunnel furnace.Also useful rotary kiln.The energy consumption height of these methods is generally at 5～15kwh/kg.The productive expense height, low comprising crucible wastage rate height and electrical heating element life-span.Aspect the employing fluidized bed reactor some progress are being arranged in recent years, as CN 86106355, adopt the rare earth oxalate after drying tangentially to be sent into by the reactor bottom side with the gas delivery method, rotation rises to top expanded section, derives reactor by the upflow tube of centre.Owing to need the rare earth oxalate of oven dry, and endotherm section is below heat release section, and latter's liberated heat can't utilize, and makes power consumption not have clear superiority, is difficult to compete with tunnel furnace under industrial condition.By this rare-earth oxalate oxidizing roasting technology and device (CN 88100388.3) with bright person invention, can directly use the draw acid rare earth of planar water, need not to dry in advance thereafter.In view of the defective of its constitutional features causes the chloride content (Cl of this system to the raw material rare earth oxalate
-) sensitivity, easily produce high temperature bond and cause defluidization.There is localized hyperthermia's band near oxidation (burning) district of the anhydrous oxalic acid rare earth the air inlet, is easy to cause the overheated of this section electrical heating element to burn.In addition, the main shaft bearing dirt exclusion capabilities difference of disk removal device easily causes " seize " phenomenon.The enforcement of above-mentioned this patent of defective effect.But the objective of the invention is to form the fluidized bed-moving-bed mixed type tubular type shaft furnace reactor oxidizing roasting system of a long-time running under industrial condition.The planar water and the chloride content of rare earth can be stood by this system, and well heater has the life-span of normal industrial furnace, and removal device also meets the trouble-free operation cycle of generalization construction machinery.Under this prerequisite, the total energy consumption level of system should be better than the present device that has existed.Yield, reactivity and additional degree of soiling meet the requirement of above-mentioned rare-earth industry.
The oxidising process of rare earth oxalate divided for two steps: the oxidation of the decomposition of crystal water and anhydrous oxalic acid rare earth is that example has following reaction with the rare earth oxalate:
La
2X
3·10H
2OCe
2X
3·10H
2OPr
2X
3·10H
2ONd
2X
3·10H
2OY
2X
3·10H
2OQ
1，kJ/mol -58.177 -923.714 -198.174 -189.631 -153.298Q
2，kJ/mol -21.388 1633.137 192.092 284.182 1110.082∑Q，kJ/mol -79.565 709.423 -6.082 94.551 -43.216∑Q，kJ/mol -0.0221 0.1971 -0.0017 0.0263 0.0120
Above-mentioned data are Q as a rule as seen
2Be on the occasion of and can offset the decomposition heat Q of crystal water
1Major part, what have still has an affluence, promptly ∑ Q be on the occasion of or a little negative value.Even but industrial practical situation are the processes that resemble the high like this heat effect of roasting Sedemesis, the taller 5～15kwh/kg CeO that reaches of energy consumption
2Promptly-6196～-18589kJ/mol Ce
2X
3H
2O is than the high n of theoretical value * 10 of this numerical value
0-n * 10
1Magnitude, its reason are that the oxidation products of rare earth oxalate is micron-sized particulate.Its unit weight is near 1g/cm
3, and the density of rare earth oxide is 5.01 (Y
2O
3)～9.17 (Yb
2O
3) g/cm
3So voidage is 80～90%, this causes the difficulty of present fixed-bed type industry stoving oven heat and mass transfer process, and under the process reaction speed, reaction heat effect is well below the thermosteresis of body of heater.The present invention takes fluidized bed reactor, has fundamentally solved the heat transfer and the mass transfer problem of micron particles material.
Fig. 1 is a device synoptic diagram of the present invention.
Contain of hopper 1 adding of the rare earth oxalate of planar water＜8% from the electric and magnetic oscillation feeder.In view of so the electromagnetic vibrator 2 of the mobile extreme difference removal device of the rare earth oxalate that contains planar water is to be operated in that its working system is that amplitude transfers to maximum under the pulse condition, the frequency of regulating impulse power supply and shake empty than to realize control to feeding quantity.Material adds by filling tube 3, and one group of desk-top baffle plate of hollow back taper is arranged in the filling tube 3, plays the labyrinth seal effect, is used to cushion the recoil of the malleation of moment to feeder.Material drops on the main file plate 3, is distributed to along its conical surface on the back taper of lower end of gravity-centrifugal settling vessel 5 to flow in the reaction tubes 17 again.Reaction tubes overcoat round shape electric heater 18, well heater be divided into 4～5 (A～E), by separately independently temperature regulator control each section temperature.There are thermal insulation layer 14 and shell to constitute electric furnace 13 outside the well heater 18.Be an annular space 16 between well heater 18 and the reaction tubes 17, make 17 not contact with 18.The coaxial installation round shape air distribution post 15 in reaction tubes middle part.Its upper edge different heights is provided with the outlet of 3～5 layer of air.Every layer of outlet is made up of equally distributed aperture.The little centerline hole post cylinder inner wall circumference that distributes therewith tangentially intersects, and has 30～45 ℃ of downward angles of depression, aperture 1～2.5mm, pitch of holes 8～15mm.Between the outlet of each layer of air is isolated mutually, and with separately independently inlet pipe 19 link.Air flows out from aperture and forms jet, and the inwall that can join reaction tubes 17 plays souring.The annular space spiral of air between reaction tubes 17 and air distribution post 15 rises and drives material and rotate.This motion has prevented the bonding of material effectively, and prolongs its residence time in bed.This 3～5 layer of air outlet is placed in the space of a well heater or two well heaters.Reaction tubes 17 extends the bottom of electric furnace 13 always and connects with the top cover of disk removal device 29 through stuffing box 26, can do free expansion downwards under breakseal state not and stretch.Removal device 29 has an airtight housing.Seal assembly 31 and 32 are arranged between main shaft 28 and housing.Disk 27 is directly installed on the main shaft 28, and its upper surface has a cone, its end footpath≤reaction caliber.The 31st, be fixed on do with one heart and mutually on the removal device base plate discontiguous nested.It is highly identical and less than the distance of disk to the removal device base plate.In moving bottom not a horizontal scraper of radial is arranged, its length has a gap less than the spacing between adjacent two set collars of this rotating ring between this scraper and the removal device housing base plate.A Kong Yuyi little pipe coupling arranged on the base plate between these two set collars.This tubule directly closely is connected with a small vessels (as plastics bag), and when powder entered space between these two set collars, horizontal scraper can be scraped it in above-mentioned small vessels, has protected main shaft bearing can not advance ash from face.An outside horizontal scraper is arranged in the lower end of disk outer fixed rotating ring, the cylindrical housing of this cutter and removal device housing and and its base plate between gapped.The powder that falls into this link can be drawn together in the relief hole that is arranged on the base plate.Relief hole is connected with drainage conduit 30, and the latter and packaging vessel are tightly linked.Guarantee that material enters in the packaging vessel continuously under the condition that is hedged off from the outer world.
At the furnace bottom of electric furnace 13 and the reaction tubes between removal device 29 loam cakes is the cooling section of furnace charge.For the little device of output (＜5kg/h), this section natural air cooling can satisfy the requirement of the temperature of charge that plastic packaging bag discharges removal device.And can take to force the refrigerative method for bigger device, and being provided with a cooling jacket 22 in outside, the extension of this regional reaction tubes, its inside is equipped with an intercooler 23, and heat-eliminating medium can be with airflow or water.The lower end of internal cooling does not contact nested with the cone of the disk of disk removal device.
Carry some dust secretly in the tail gas that roasting process produces.This dust-laden tail gas directly enters the gravity-centrifugal dust collector that connects with it after outflow reactor is suitable for reading, make the first step and handle.In view of micronic dust material particle is tiny, general gravitational settler efficient is low, so two kinds of plate washers are installed in this settling vessel, it is mobile that air-flow is turned back, and promptly increases a part of centrifugation, to improve dust-collecting efficiency.Air-flow enters settling vessel, stopped by main file plate 8, enters the venetian blind type plate washer group 10 that is installed in above the main file plate 8 then.This plate washer group is made up of the hollow back taper stage body that a cover can be nested each other.Air-flow flows through the generation fold return motion the gap between two adjacent plate washers.For preventing that air-flow from directly entering vapor pipe 12.Outside the plate washer group 10 gas hood 7 and 6 are arranged, make most of dusty gas force to enter plate washer group 10.Microfarad under deposition on the gas hood 7 flows into the bottom of settling vessel along under its conical flow from the slit between the cylindrical housing of its lower edge and settling vessel, join with the micronic dust that settles down in the venetian blind type plate washer group 10 and return in the reaction tubes 17 along wall.The vapor pipe 12 of this gravity-centrifugal settling vessel connects with coming level back flushing type bag filter.For guaranteeing that bag filter is operated in more than the dew point of tail gas and is lower than the upper limit of cloth bag working temperature, has a heat exchanger 11 on vapor pipe 19.On the little device of output (≤5kg/h), coated thermal insulation layer is lower than the dew point of tail gas with the temperature that prevents the bagroom ingress.For than bigger device (〉=10kg/h), adopt the naked pipe natural air cooling or adopt forced air cooling or water-cooled with cooling jacket, be not higher than cloth bag with the temperature at place, control bagroom gas inlet and allow maximum operating temperature.Under the situation of burning carbon acid rare earth, in view of not anti-thermal response in the roasting process, effusive dust-laden exhaust temperature is very low from gravitational settler, near room temperature, far below the dew-point temperature of tail gas.In order to guarantee＜ask legal use software〉works better of bag collector, the interchanger 11 on vapor pipe should be an electric heater, makes the gas inlet temperature of bagroom be higher than the dew-point temperature of tail gas.The operating temperature range of above-mentioned bagroom is 80～150 ℃.
When this unit normal run, material is in fluidized state in the central column space between distribution post 15 and reaction tubes 17 more than the basecoat pelvic outlet plane of air distribution post 15.Usually the charge level of fluidized bed is at the 300～600mm place more than the last layer pelvic outlet plane of distribution post 15.This charge level is generally in the relative place of B well heater.The freeboard of fluidized bed of forming by the particulate that blows out and 17 inwalls flow down from gravitational settler 5 along reaction tubes particulate and raw material more than the charge level.The agglomerating particles of raw material and half point hydrolysis products is owing to the particulate of its granularity greater than material in the fluidization bed, so sink to below the charge level, but＜please legal use software spiralling air-flow and particulate media clamping, descend slowly, meanwhile carry out violent heat exchange with medium, remove the reaction of planar water and crystal water, carry out preheating simultaneously.Show along the short transverse thermograde little from temperature distribution.The temperature of freeboard of fluidized bed is 700～800 ℃.Charge level is being 800～900 ℃ down to the first layer air place.The control discharge velocity can fully be finished material and is removed planar water and crystal water in these two intervals, material is made up of the anhydrous oxalic acid rare earth.After the anhydrous oxalic acid rare earth that is preheated enters the airstream district, begin " having lighted " immediately, carry out similar incendiary oxidizing reaction.Material discharges a large amount of heats here, and the temperature that makes zone of combustion rises by the thermograde of 8～9 ℃/cm and reaches 900～1050 ℃.The top temperature of zone of combustion exceeds 15～20 ℃ than the reference mark.Furnace charge passes the strong oxidation zone of being made up of the outlet of 3～5 layer of air can finish oxidising process substantially.Mainly form at the following material of orlop air by the pyritous rare earth oxide, because from coiling the removal device to the garden here is a stock column of being made up of this material, form the material envelope, so operation along with removal device, material is constantly discharged, new material constantly flows out from fluidized-bed and replenishes, and making becomes moving-bed here.In the above 0.5m of furnace bottom, still there is a small amount of intermediate product that does not decompose fully to carry out thermolysis there.This structure can make reactivity＞99%.
Be two embodiments of the present invention below.
One: one of example is pressed designed system of the present invention.Reaction tube diameter 440mm, reaction tubes and air distribution post are made by Refractoloy, the outlet of three layer of air, four sections well heaters.Input igloss is 68.53% Sedemesis 1890.50kg in 48 hours, and output igloss is 0.25% cerium oxide (CeO
2).By the micronic dust 78.60kg that bagroom reclaims, its igloss is 4.18%.Because charge level raises than before demarcating, many accumulation 40kgCeO in the system
2Total power consumption 1462.5kWh.
Reaction tube diameter is 225mm to two: one of examples by designed system of the present invention, the outlet of three layer of air.Reaction tubes and air distribution post are made of the nickel-base high-temperature refractory alloy, four sections well heaters.Input igloss is 64.53% praseodymium oxalate 2219kg in 296.3 hours, amounts to Pr
6O
11786.8kg.The output finished product is amounted to Pr
6O
11709.1kg igloss is 0.05%, residue bagroom ash is amounted to Pr
6O
1151kg, other has 26kg to be stranded in the system.Average current drain 4.2kWh/kgPr
6O
11NiO content in the product increases 44ppm than praseodymium oxalate.
Claims (14)
1. one kind is carried out oxidizing roasting or the method for roasting particle shape material production micropowder material in neutral atmosphere in fluidized bed-moving-bed mixing bed, it is characterized in that granular material is carried out roasting in the system of a riser type reactor with ring section that includes built-in cylindrical gas distribution post, the pneumatic outlet of this cylindrical gas sparger is at the middle part of reactor, gas is by the hand of spiral rising of spiraling, stock column more than the pneumatic outlet plane is in fluidized state, wherein charge level is following is the bubbling bed, it on it dust freeboard of fluidized bed, the bottom of bubbling bed is 900～1050 ℃ of high-temperature zones, its top and dust freeboard of fluidized bed are 700～900 ℃ middle warm areas, be moving-bed below the bubbling bed, as cooling section, material is continuous flow from top to bottom, warm area preheating dehydration in the ingress of reactor enters with the mix dust of returning, enter the high-temperature zone then and carry out oxidation or carry out pyrolysis, solid product is discharged continuously through cooling section.
2. method according to claim 1 is characterized in that the dusty gas product that takes place reclaims through dust-precipitator, again Returning reactor in the riser type reactor of ring section.
3. method according to claim 1, what it is characterized in that handled granular material first-selection is rare-earth oxalate and the carbonate that contains planar water＜8%, to produce rare earth oxide.
4. system that implements the roasting of the described method of claim 1, it is characterized in that it being this roasting system, be by round shape reaction tubes (17) and with the riser type fluidized bed-moving-bed mixing reactor of its cylindrical gas distribution post (15) institute makeup ring tee section of installing with one heart, gravity-centrifugal dust collector (5), bagroom, electric and magnetic oscillation feeder (1,2), garden dish dumper (29) and air-supply, induced draught system are formed.
5. system according to claim 4 is characterized in that the difference Δ D of the external diameter of the internal diameter of said round shape reaction tubes (17) and cylindrical gas distribution post (15) should be satisfied with 60≤Δ D≤150mm.
6. system according to claim 4, the surperficial upper edge axis direction that it is characterized in that said gas distribution post (15) is provided with 2～5 layers of pneumatic outlet (20) on different heights, each interlamellar spacing is 150～300mm, orlop is apart from reactor bottom＞0.5m, every layer of pneumatic outlet by in the garden on week equally distributed aperture formed by the aperture of 1～2.5mm, pitch of holes 8～15mm, little centerline hole cylindrical gas distribution column wall circumference therewith tangentially intersects and has a downward angle of depression of 30～45 °, between each layer pneumatic outlet on gas circuit be mutually isolated and with separately independently intake ducting be connected, intake ducting can be introduced from the top of reactor, also can introduce from the bottom of reactor.
7. system according to claim 4, the gas that it is characterized in that said feeding gas distribution post (15) is air or rare gas element, and the material of round shape reaction tubes (17) and cylindrical gas distribution post (15) is quartz, diamond spar, Refractoloy or at the Refractoloy of surperficial spray aluminum oxide or rare earth oxide.
8. system according to claim 4, riser type fluidized bed-moving-bed the mixing reactor that it is characterized in that said ring section is installed in the round shape vertical electric furnace (13) of a multistage heating with one heart, every section has independently power supply and temperature control system, can form certain temperature field in reactor according to processing requirement.
9. system according to claim 4, the shell upper that it is characterized in that said gravity-centrifugal dust collector (5) is a garden tube, it is connected with the inversed taper platform of a hollow down, the latter's end opening is connected with the suitable for reading of reactor, as inlet mouth, the taper main file plate (8) and the multiple damper group (10) of a hollow upwards are installed thus successively, the latter is made up of the hollow back taper stage body that a cover can be nested each other, and these baffle group are placed in hollow frustum (7) and the gas hood (6).(7) and the passage that has the dust Gong collecting to flow down between the inwall of shell.
10. system according to claim 4, it is characterized in that said gravity-centrifugal dust collector (5) is provided with a charging opening at its top, be connected with a filling tube (3), this filling tube passes the top of multiple damper group (10) to taper master shield (8), its inside can be provided with multilayer hollow inversed taper platform shape baffle plate (4), form maze-type structure, charging opening can be installed in the side of dust-precipitator where necessary, can contain the horizontal duct of a baffle maze group by an inside, its outlet is located between master shield on the central axis and multiple damper group.
11. system according to claim 4, it is characterized in that said its electric and magnetic oscillation feeder (1,2) be made up of power frequency electromagnetic vibrator (2), hopper (1) and horizontal duct, the source of power frequency electromagnetic vibrator is through adjustable pulsating direct current of the voltage of half-wave rectification or frequency and shakes empty than adjustable pulsed current.
12. system according to claim 4, it is characterized in that the shell of bagroom with a well insulated, its working temperature is 80～150 ℃, and has the pulse purging system.
13. system according to claim 4, it is characterized in that gravity-centrifugal dust collector and the connecting tube between the bagroom (12) be an interchanger, according to the heat of discharging gas can be water cooler, can be electric heater, also can be thermal insulation layer.
14. system according to claim 4, the outlet that it is characterized in that said reactor is connected with a closed garden disc type removal device (29), reaction tubes directly stretches in the cylinder of an internal diameter greater than the outer warp of round shape reaction tubes that covers on the removal device, there is a stuffing box (26) on the top of this cylinder, make sliding sealing with reaction tubes, the support of bearing top of disk is higher than the loam cake of garden disc type removal device, labyrinth type dustproof ring group is being arranged below the disk and between the bottom, a pair of above cylinder is arranged, awl tube or the mixed structure of the two, each is fixed on (32) on the disk to one in the tube, another is fixed on, and (31) do not contact nested forming mutually on the base plate, there are being an openable hole and one to be fixed on the disk the cutter of drawing together on the relative position with it on the base plate between two sleeves that are fixed on the base plate, draw together the cutter edge of a knife apart from base plate～1mm, the drive-motor of disk is operation or intermittent operation continuously, and drainage conduit and packing bag are tightly connected.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94116925A CN1039593C (en) | 1994-10-14 | 1994-10-14 | Calcining system and technique for fluidized bed-mobile bed mixed reactor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94116925A CN1039593C (en) | 1994-10-14 | 1994-10-14 | Calcining system and technique for fluidized bed-mobile bed mixed reactor |
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| Publication Number | Publication Date |
|---|---|
| CN1120588A CN1120588A (en) | 1996-04-17 |
| CN1039593C true CN1039593C (en) | 1998-08-26 |
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|---|---|---|---|
| CN94116925A Expired - Fee Related CN1039593C (en) | 1994-10-14 | 1994-10-14 | Calcining system and technique for fluidized bed-mobile bed mixed reactor |
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| CN103409615B (en) * | 2013-07-29 | 2014-09-10 | 青岛智邦炉窑设计研究有限公司 | Mineral roasting reduction device and application method thereof |
| CN104846194B (en) * | 2015-03-16 | 2017-08-04 | 北京矿冶研究总院 | Cooling method of chloridized roasted pellets |
| CN105419877B (en) * | 2015-12-21 | 2018-02-27 | 代建军 | Two sections of pyrolysis gasification systems of solid waste based on fluid bed and moving bed |
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| CN115790229B (en) * | 2023-02-13 | 2023-05-09 | 成都天保节能环保工程有限公司 | Heat storage method suitable for fluidized bed heat storage structure |
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