CN2257496Y - Spray pyrolytic device for preparing hollow tiny powder material - Google Patents
Spray pyrolytic device for preparing hollow tiny powder material Download PDFInfo
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- CN2257496Y CN2257496Y CN96212116U CN96212116U CN2257496Y CN 2257496 Y CN2257496 Y CN 2257496Y CN 96212116 U CN96212116 U CN 96212116U CN 96212116 U CN96212116 U CN 96212116U CN 2257496 Y CN2257496 Y CN 2257496Y
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Abstract
The utility model relates to a spray pyrolyzing device for preparing hollow tiny powder materials. The utility model is characterized in that a gas inlet pipe 1 of an atomizer 7 is consolidated with a gas and liquid mixing pipe 2; a liquid inlet pipe 3 arranged on the contraction part of the lower part of the gas and liquid mixing pipe 2 is consolidated on the contraction part of the gas and liquid mixing pipe 2 and is perpendicular to the gas and liquid mixing pipe 2; the gas and liquid mixing pipe 2 is connected with a throat pipe 5 of the atomizer by threads, and a sealing sleeve 4 is arranged in the gas and liquid mixing pipe 2; the atomizer throat pipe 5 is consolidated with a bell cover-shaped dilation pipe 7 into a whole; a floating ball 6 is arranged on the throat of the throat pipe 5 of the atomizer. The utility model has the advantages of high atomization efficiency, low power consumption, plugging resistance, continuous operation, etc.
Description
The utility model relates to a kind of spray pyrolysis unit, relates in particular to a kind of spray pyrolysis unit for preparing hollow fine powder material.
Produce the common used method of fine powder material and solid phase method is arranged, coprecipitation, citric acid method, drip pyrolysismethod, glycine-nitrate process etc.
Powder with solid phase method preparation need pass through long-time ball milling, thereby introduces impurity easily, powder size more than 1 μ m and uniformity relatively poor, sample sintering temperature height and be easy to generate dephasign.
Coprecipitation has powder particle tiny (can reach 0.3 μ m), mixes, and the surface-active height, solid phase reaction is complete, and the sample sintering temperature is low, densification, advantage such as stable performance and repeatability are good, but preparation process also must be passed through ball milling.PH value in the precipitation process needs accurately control, also has problems such as precipitation is incomplete simultaneously.
The powder size of citrate synthetic method preparation is little, and the reunion degree is lower, and required sintering temperature is also lower, but needs the pH value of strict control solution in the preparation process, needs condition of ice bath, and cost is also higher.High-temperature calcination easily causes the hard aggregation of powder, still need be through grinding before the use.
The advantage of drip pyrolysismethod is that prepared powder single phase property is good, and the metallic element homogeneous distributes.The drip pyrolysismethod has important disadvantages: the one, because charging rate is subjected to restriction capillaceous, thereby output is very little, and is difficult to amplify; The 2nd, because product is among the high temperature always, the particle agglomeration is serious, and the particle diameter of agglomerated particle can reach 500 μ m; The 3rd, reaction may be emitted a large amount of pernicious gases, causes environmental pollution.
Glycine-nitrate process method [1]: preparation technology is fairly simple.When the proportioning of fuel/oxidant was appropriate, natural reaction can be finished in moment.The temperature of combustion flame can be between 1100 ℃ to 1450 ℃ with the difference of nitrate/glycine proportioning (N/G).By regulating suitable N/G proportioning, can generate H
2O, CO
2, N
2Deng gaseous product, thereby can avoid the NO that is harmful to
2Generate.But fume amount is big, and operating condition is abominable, and the process direct yield is lower.
Above-mentioned the whole bag of tricks all belongs to intermittent operation, and batch output is lower, is difficult to realize scale, serialization production industrial.
Adopt spray pyrolysis, can continued operation, be expected to realize industrial scale and serialization, be applied to Al
2O
3The preparation of powder.But the nebulization efficiency of existing pyrolysis oven is low, and what need is large-minded, and energy consumption is big; Furnace is difficult to control; Residence time of material is short, decomposes not exclusively.For this reason, the utility model has adopted new design.
The spray pyrolysis process:
Raw materials usedly can be the easily oxysalt of pyrolysis, the organic metal ionic complexing agent and (or) mixed solution of volatile easy firing material.Material liquid enters pyrolysis oven with certain speed after the atomizer atomizing.Along with temperature raises, solute is together separated out in company with the organic metal ionic complexing agent, form the solid gel particle of doing.The gel particle intensification that continues to be heated, when heat to 200 ℃, because the temperature instability of oxysalt and strong oxidisability, pyrolytic reaction takes place, emit oxygen, make flammable organic metal ionic complexing agent burning, oxysalt forms oxide powder, and the organic metal ionic complexing agent forms water and nontoxic gas cyaniding thing.The chemical composition of product is determined by the institute that forms of precursor liquid.The crystalline state of product becomes by the forming of precursor liquid, pyrolysis temperature, reaction time etc. to be determined.
The purpose of this utility model provides a kind of nebulization efficiency height, less energy consumption, is difficult for stopping up, but continued operation can realize the spray pyrolysis unit of the hollow fine powder material of preparation of industrial scale and serialization.
The concrete solution of the utility model is: a kind of spray pyrolysis unit for preparing hollow fine powder material, comprise: air compressor machine 1, Pressure gauge 2, control valve 3, flowmeter 4, hopper 5, wriggle and flow pump 6, atomizer 7, controllable silicon temperature controller 8, thermoelectric pot 9, pyrolysis oven 10, pyrolysis oven 11, heat exchanger 12, cottrell 13, clear water head tank 14, leacheate head tank 15, packed absorber 16, vent gas treatment tower 17, it is characterized in that: atomizer 7 comprises: gas inlet pipe 1, gas-liquid mixed pipe 2, feed liquid input pipe 3, sealing shroud 4, atomizer trunnion 5, ball float 6, bell shape convergent divergent channel 7, wherein, gas inlet pipe 1 and gas-liquid mixed pipe 2 concrete mutuallies; One contraction place is arranged at gas-liquid mixed pipe 2 bottoms, and feed liquid input pipe 3 is cemented in the contraction position of gas-liquid mixed pipe 2 and vertical mutually with gas-liquid mixed pipe 2; Gas-liquid mixed pipe 2 be connected with atomizer trunnion 5 spiral shells and in sealing shroud 4 is arranged, atomizer trunnion 5 is consolidated into one with bell shape convergent divergent channel 7; Ball float 6 is arranged on the aditus laryngis place of atomizer trunnion 5.The electric furnace heating wire of pyrolysis oven ten along furnace outer wall in the shape of a spiral tubulose to the winding of enclosing the land of the other end one of flue, its twine spacing by close to rare.Pyrolysis oven 11 is along the furnace outer wall uniform winding.
Advantage of the present utility model and good effect are:
1. adopt novel atomising device, can produce the droplet of 0.01 μ m; The self-cleaning effect is arranged, be difficult for stopping up; Required tolerance is few, energy savings; The time that material stops in stove is long, and pyrolytic reaction is complete.
2. be provided with the bell shape convergent divergent channel, make fog concentrated relatively, thereby can require less furnace diameter.
The bell shape convergent divergent channel is the droplet of recyclable sedimentation also, makes product granularity even.
3. atomizer arrangement can not guaranteed atomizer running steady in a long-term by high-temperature baking in the lower end of body of heater.
4. enclosed type body of heater, product can not polluted.
5. simple in structure, cost of investment is low.
6. production process serialization, with short production cycle.
Spray pyrolysis unit
Device connection diagram of the present utility model as shown in Figure 1, by air supply system, feeding system, temperature control system, atomizer, pyrolysis oven, heat exchanger, product gathering system and exhaust treatment system are formed.
1. air supply system: by air compressor (1), Pressure gauge (2), valve (3), flowmeter (4) is formed.
The pressure that air compressor provides is adjustable in 0-10atm (gauge pressure) scope.
2. feeding system: by hopper (5), peristaltic pump (6) is formed.
3. heat supply and temperature control system: by power supply, controllable silicon temperature controller (8), thermocouple (9) is formed.
4. ball float atomizer
The kind of atomizer is a lot, mainly contains rotary atomizer and nozzle atomization device.Though different atomization techniques adopts multi-form energy to feed liquid, they all are to utilize energy that feed liquid is disperseed.The two mixed type ball float atomizers of the present utility model, as shown in Figure 2.It is few that it can satisfy institute's air demand, the requirement that droplet is thin and concentrated.It is by gas inlet pipe (1), gas-liquid mixed pipe (2), and feed liquid input pipe (3), sealing shroud (4), ball float atomizer trunnion (5), ball float (6) and bell shape convergent divergent channel (7) are formed.The gas-liquid mixed pipe is that a straight person in charge manages with the T shape that a vertical with it other pipe is formed, the straight tube ventilation, the logical feed liquid of other pipe, feed liquid straight tube shrink that suction that the bore place produced by high velocity air aspirates and in straight tube by the gas whirlpool fragmentation, atomize by the slit between atomizer trunnion and the ball float then, ball float constantly trembles, and the self-cleaning effect is arranged; Ball float can be avoided fog directly to dash to the outlet of burner hearth upper end and cause short circuit.The size of droplet is easy to the ball float that varies in weight by replacing and regulates gas/liquid and recently regulate.Bell shape convergent divergent channel (7) can make fog concentrate, and avoids wet fog to drip directly being sprayed onto hearth wall and causes and scab, thereby can adopt the less burner hearth of diameter, saves investment and makes in the burner hearth temperature field even; Big droplet also can flow back into its throat and be atomized once more, makes product granularity more even.This atomizer structure is simple, and is less demanding to stream pressure, and required tolerance is few, guarantees that material has the sufficient time of staying in stove.Can handle the high viscosity feed liquid.Its physical dimension is as follows
Gas-liquid mixed pipe straight tube: material stainless steel tube, internal diameter 5-20mm, contraction place internal diameter 3-10mm, length 50-200mm
The other pipe of gas-liquid mixed pipe: material is a stainless steel tube, internal diameter 3-10mm
Ball float (6): material is stainless steel or pottery, diameter 10-25mm
Trunnion (5): material is stainless steel or pottery, diameter 5-20mm
Bell shape convergent divergent channel (7): 15-60mm
This type of atomizer is not seen both at home and abroad report.
5. pyrolysis oven
Two of pyrolysis oven employings or many tube type resistance furnaces are in series, and the cross over pipe between each stove will be incubated.Each furnace height is 1400-2000mm.Wherein first stove is that droplet concentrates and pyrolysis oven, and second later stove is the crystal formation reburner.
Stove is by flue, electric furnace heating wire, and heat-insulation layer, furnace shell is formed.Flue is the very smooth earthenware of inner surface.Bore is 60-300mm, decides on the output size.Body of heater is vertically installed, and atomizer is installed in the stove lower end, and atomizer can not warmed by the hot gas of stove like this, guarantees atomizer operation steady in a long-term.The big drop of coalescence can reflux, and can not form block.
The furnace temperature of each stove relies on electric heating to keep, and each stove is respectively with a controllable silicon temperature controller control temperature.Electric furnace heating wire is begun by an end of flue, along furnace outer wall in the shape of a spiral tubulose to the winding of enclosing the land of the other end one of flue.At a certain distance, with ceramics two adjacent circle electric furnace heating wires are separated, and fix with high-temperature flame-proof mud.
Wherein Temperature Distribution relies on the porousness of electric furnace heating wire to realize in the stove of first stove.The difference of product form and different arrangement the as requested.Micro mist is a hollow ball shape, and electric furnace heating wire should be by close thinning from top to bottom for first electric furnace.The upper semisection furnace temperature will be controlled in a little higher than feed liquid decomposition temperature of difficult decomposition components.
The temperature of second and all the other each stoves should maintain the desired temperature of crystal transfer.Temperature requirement is even in the stove, so the furnace outer wall electric furnace heating wire is answered uniform winding.
System's micro-pressure operation, pressure is regulated by the air exhauster of equipment afterbody.System is closed, can prevent the pollution of impurity like this, does not influence the continuity of production again.
This type of pyrolysis oven is not seen both at home and abroad report.
6. heat exchanger: purpose is the cooling furnace gas, in order to avoid high-temperature furnace gas damages the product gathering system, utilize burner gas residual heat preheated air and feed liquid simultaneously again, improve the temperature of going into the stove air as far as possible, make feed temperature near 100 ℃, thus but energy savings and quickening reaction in furnace speed.The utility model adopts blade heat exchanger, reverse-flow operation.
7. product gathering system
The means that adopt clean cottrell and packed tower wet dust collector to combine are collected micro mist.
The washing of packed tower adverse current, filler tower height 910mm, inner stuffing are particle diameter 2-3mm glass marble, packed height is 740mm.
8. exhaust treatment system
Adopt lime cream absorption method to handle tail gas.
Mutual connection adopting quartz glass pipe, glass tube, earthenware or the stainless steel tube of device each several part
The operating procedure of pyrolysis oven:
(1) preparation precursor solution
(2) pyrolysis oven is warming up to preset temperature, guarantees that with the controllable silicon temperature controller furnace temperature is constant.
(3) open heat exchanger.
(4) in packed tower, add deionized water, and make liquid level exceed filler 20-50mm.
(5) start cottrell.
(6) start air compressor, make its constant pressure at 4.0Kgf/cm
2
(7) regulate the spinner flowmeter knob, the throughput that control enters atomizer.
(8) start the stream pump of wriggling, thereby regulate charging knob control feed liquid flow.
(9) regularly from electrostatic precipitator and packed tower, collect micro mist.
(10) cleaning solution is carried out suction filtration, the filter cake that obtains is in 100-108 ℃ of following freeze-day with constant temperature.
Fig. 1 is the utility model device connection diagram.
Fig. 2 is the structural representation of the utility model atomizer 7.
Fig. 3 is the SEM photo of the prepared powder of the utility model temperature contrast experiment.
Fig. 4 is the SEM photo of the prepared powder of the utility model concentration contrast experiment.
Fig. 5 is the XRD spectra of the utility model product.
Fig. 6 is for using the SEM photo of the made powder of the utility model.
Below in conjunction with accompanying drawing the utility model is further described.
A kind of spray pyrolysis unit for preparing hollow tiny powder material comprises:
Embodiment one:
Mix strontium lanthanum manganate La
0.8Sr
0.2MnO
3Preparation (20LSM)
(1) influence of pyrolysis temperature
Along with the rising of pyrolysis temperature, powder size is the trend of increase, sees Table 1.
Table 1 pyrolysis temperature is to the influence of powder size
Temperature (℃) 450 500 550 600 650 particle mean sizes (μ m) 0.609 0.689 0.673 0.779 0.879
In order further to determine the influence of temperature, be that 0.6M, gas/liquid ratio are 9.16 * 10 in solution concentration to powder size
3, nitre/sweet ratio is under 1: 1 the condition, to carry out following contrast experiment, the result is as follows:
(1)T＝500℃， d＝0.667μm；
(2)T＝700℃， d＝1.383μm；
Prepared powder is seen photo (1) and (2) among Fig. 3 respectively.As seen, temperature raises, and the particle mean size of powder obviously increases.
(2) influence of gas/liquid ratio
Along with the increase of gas/liquid ratio, powder size reduced before this gradually, became big then again suddenly.The result is as shown in table 2.
Table 2 gas/liquid ratio influences gas/liquid ratio (* 10 to powder size
-3) 3.56 5.00 9.16 11.77 15.31 particle mean sizes (μ m) 0.751 0.647 0.733 0.621 0.874
(3) influence of concentration of raw material
By table 3 as seen, along with the increase of feed concentration, powder size increases earlier gradually, is tending towards again then reducing.
Table 3 feed concentration influences feed concentration (M) 0.2 0.4 0.6 0.8 1.0 particle mean sizes (μ m) 0.74 10.769 0.83 10.66 10.627 to powder size
In order further to determine the influence of feed concentration, be that 550 ℃, gas/liquid ratio are 9.16 * 10 in temperature to powder size
3, nitre/sweet ratio is under 1: 1 the situation, to be following contrast experiment:
(1)C＝0.2M，d＝0.600μm；
(2)C＝1.0M，d＝0.433μm；
The prepared powder of contrast experiment is seen (1) and (2) among Fig. 4 respectively.
Embodiment two: the physico-chemical property of 20LSM powder
(1) chemical composition of powder,
With the powder that obtains in Muffle furnace after fusing 2.5hr under 1150 ℃, analyze with EDAX, the result who obtains is as shown in table 4.
Content (a/o) La: Sr: the Mn of the content No. element of element in table 4 powder
La Sr Mn1. 39.34 10.91 49.75 0.791∶0.219∶12. 41.09 9.65 49.26 0.834∶0.196∶1
Annotate: data obtain with the EDAX method in the table
(2) crystal structure of powder:
With the crystal formation and the phase composition of X-ray diffraction method mensuration powder, the powder that discovery is prepared from pyrolysis oven, through the powder of 1150 ℃ of roastings, crystal formation is six sides--the diamond pattern crystallographic system.The structure of this moment is very similar to the standard spectrum (JCPDS32--484) of LaMnO3.15, does not almost have unnecessary spectral line, and single phase property is very good, as shown in Figure 5.
(3) electrical property of ultra micro powder:
In order clearly to use the La that spray pyrolysis is prepared
0.8Sr
0.2MnO
3(20LSM) resistance of sample is tested.With the 20LSM powder on universal hydraulic testing machine with 2.5 tons/cm
2Pressure be pressed into base, cool off with stove behind the insulation 3.0hr. down in 1150 ℃.Specimen finish is 18.66mm, thick 2.36mm.Adopt Pt to go between, two lead-in wires are fixed on two surfaces of sample.Sample is placed in the Muffle furnace, in 50-1200 ℃ temperature range, carry out the test of resistance (R), and calculate electrical conductivity thus.Along with temperature raises, the almost linear increase of the resistance of sample.Can infer that thus sample is the metallic conduction type.
Embodiment three: optimum operation condition
The spray pyrolysis Orthogonal experiment results is carried out variance analysis, has determined that optimum experimental condition is:
Concentration 1.0M
450 ℃ of temperature
Gas/liquid ratio 11.77 * 10
3
Nitre/sweet ratio 1.4: 1
When selecting optimum process condition for use, powder size drops on possibility between the 0.016-0.639 μ m more than 95%.The particle mean size of the powder among Fig. 6 (1) is 0.244 μ m, and the particle mean size of the powder among Fig. 6 (2) is 0.275 μ m.
Claims (2)
1, a kind of spray pyrolysis unit for preparing hollow fine powder material, comprise: air compressor machine 1, Pressure gauge 2, control valve 3, flowmeter 4, hopper 5, wriggle and flow pump 6, atomizer 7, controllable silicon temperature controller 8, thermocouple 9, pyrolysis oven 10, pyrolysis oven 11, heat exchanger 12, cottrell 13, clear water head tank 14, leacheate head tank 15, packed absorber 16, vent gas treatment tower 17, it is characterized in that: atomizer 7 comprises: gas inlet pipe 1, gas-liquid mixed pipe 2, feed liquid input pipe 3, sealing shroud 4, atomizer trunnion 5, ball float 6, bell shape convergent divergent channel 7, wherein, gas inlet pipe 1 and gas-liquid mixed pipe 2 concrete mutuallies; One contraction place is arranged at gas-liquid mixed pipe 2 bottoms, and the contraction flow regions that feed liquid input pipe 3 is cemented in gas-liquid mixed pipe 2 are vertical mutually with gas-liquid mixed pipe 2; Gas-liquid mixed pipe 2 be threaded with atomizer trunnion 5 and in sealing shroud 4 is arranged, atomizer trunnion 5 is consolidated into one with bell shape convergent divergent channel 7; Ball float 6 is arranged on the aditus laryngis place of atomizer trunnion 5.
2, a kind of spray pyrolysis unit for preparing the fine powder material according to claim 1 is characterized in that: the electric furnace heating wire of pyrolysis oven 10 outside flue the amount of keeping away helix to the winding of enclosing the land of the other end one of flue, its twine spacing by close to rare.Pyrolysis oven 11 is along the furnace outer wall uniform winding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96212116U CN2257496Y (en) | 1996-05-29 | 1996-05-29 | Spray pyrolytic device for preparing hollow tiny powder material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96212116U CN2257496Y (en) | 1996-05-29 | 1996-05-29 | Spray pyrolytic device for preparing hollow tiny powder material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2257496Y true CN2257496Y (en) | 1997-07-09 |
Family
ID=33894876
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96212116U Expired - Fee Related CN2257496Y (en) | 1996-05-29 | 1996-05-29 | Spray pyrolytic device for preparing hollow tiny powder material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2257496Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419879A (en) * | 2015-11-05 | 2016-03-23 | 东华工程科技股份有限公司 | Device and method for catalytically decomposing coal substances and separating coal substances at high temperatures |
| CN106225515A (en) * | 2016-09-13 | 2016-12-14 | 成都创慧科达科技有限公司 | A kind of tandem flue gas heat recovery system |
-
1996
- 1996-05-29 CN CN96212116U patent/CN2257496Y/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419879A (en) * | 2015-11-05 | 2016-03-23 | 东华工程科技股份有限公司 | Device and method for catalytically decomposing coal substances and separating coal substances at high temperatures |
| CN105419879B (en) * | 2015-11-05 | 2020-07-10 | 东华工程科技股份有限公司 | Device and method for catalytic decomposition and high-temperature separation of coal substances |
| CN106225515A (en) * | 2016-09-13 | 2016-12-14 | 成都创慧科达科技有限公司 | A kind of tandem flue gas heat recovery system |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |