CN106362657A - Reaction device and method for preparing superfine rare earth compound through same - Google Patents
Reaction device and method for preparing superfine rare earth compound through same Download PDFInfo
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- CN106362657A CN106362657A CN201610799265.1A CN201610799265A CN106362657A CN 106362657 A CN106362657 A CN 106362657A CN 201610799265 A CN201610799265 A CN 201610799265A CN 106362657 A CN106362657 A CN 106362657A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J19/24—Stationary reactors without moving elements inside
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/005—Feed or outlet devices as such, e.g. feeding tubes provided with baffles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
- C01F17/271—Chlorides
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- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/276—Nitrates
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- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/282—Sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F2025/91—Direction of flow or arrangement of feed and discharge openings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F2025/91—Direction of flow or arrangement of feed and discharge openings
- B01F2025/913—Vortex flow, i.e. flow spiraling in a tangential direction and moving in an axial direction
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a reaction device and a method for preparing a superfine rare earth compound through the same. The reaction device comprises an end cover (1), at least two feeding pipes (2), a cylinder (3), a discharging port (4) and nozzles (5); the feeding pipes stretch into the cylinder (3), and the nozzles (5) are installed at the tail ends of outlets of all the feeding pipes (2); one end of the cylinder (3) is connected with the end cover (1), the other end of the cylinder (3) is connected with the discharging port (4), and the cylinder (3) is in sealed connection with the end cover (1) and the discharging port (4). According to the method, rare earth feed liquid and a precipitator are pumped into the reaction device through the different feeding pipes (2) respectively to react quickly, and the superfine rare earth compound is obtained. The reaction device is small and simple in structure, convenient to make and use, quite suitable for fluid mixing, dispersion, precipitation reactions and other tests or production and easy to clean, and can be used independently or in a combined mode.
Description
Technical field
The present invention relates to a kind of reaction unit, and the method preparing superfine rare-earth compound using this device, belonging to
Construction equipment and production technical field.
Background technology
It is often necessary to carry out the reactions such as some mixing, dispersion or precipitation in chemical field, these reactions most of one
Carry out in large-scale or more complicated equipment a bit, reach the reaction purpose of mixing, dispersion or precipitation by stirring.
In Chemical Manufacture, a kind of conventional consersion unit is that reactor is widely used in oil, chemical industry, rubber, agriculture at present
The type of production user such as medicine, dyestuff, medicine, food and the research of various scientific experiment project, for complete hydrolysis, neutralization, crystallization,
The container of the technical processs such as distillation, evaporation, storage, hydrogenation, hydrocarbonylation, polymerization, condensation, heating mixture, isothermal reaction.Reactor bag
Include kettle and agitating device, be highly suitable for the reactions such as mixing, dispersion or precipitation, by joining with parameter to the structure design of container
Put, realize heating, the mixture function of evaporation, cooling and low high speed of technological requirement.But reactor also has its obvious shortcoming:
Volume is big, needs operating platform for installing and operating, part is installed and replacing all ratios are relatively time-consuming, and cleaning also will spend more people
Power and time.
Another kind of common equipment for fluid mixing is blender, and small volume is easy to install and use, such as static
Blender, Venturi tube etc..This kind of fluid mixing apparatus, internal structure complexity, it is not easy to cleaning, is only suitable for some liquid
The aspects such as the mixing of material, emulsifying, are not suitable for precipitation, and typically special thing is special, easily cross-contamination if using with.
In terms of the preparation of rare earth material, a preparation method always difficult problem for superfine rare-earth compound.Common preparation
Method is precipitation in enamel reaction still, stops particle agglomeration by strong stirring and grows up, but precipitate is in a kettle.
Retention time is long, and granule is easily grown up, and d50 is difficult to accomplish less than 2 μm, does not reach micropowder and requires, and particle size distribution is not yet
Enough concentrations.Some specific process such as the use hydro-thermal method also having or combustion method, these methods have the characteristics that common it is simply that will
Use special installation, and process conditions complexity is not easily controlled, and is substantially all and is in laboratory stage, for realizing industrialization
Production requirement is higher.Method made above, all more or less being limited by place capacity of yield.
Content of the invention
For solving above technical problem, the present invention provides a kind of reaction unit, and this apparatus structure is compact simple, makes and makes
With conveniently, end cap can arbitrarily be erected on the containers such as reactor, filter tank, charging basket, it is very suitable for fluid mixing, dispersion, sinks
Test or the industrialized production such as shallow lake reaction, and easily clean, use manpower and material resources sparingly.
The present invention is achieved by the following technical solutions:
A kind of reaction unit is it is characterised in that include end cap 1, feed pipe 2, cylinder 3, discharging opening 4 and nozzle 5；Described enter
Expects pipe 2 at least 2, is respectively protruding in cylinder 3, and the outlet ends of each feed pipe 2 are equipped with nozzle 5, cylinder 3 one end and end cap 1
Connect, another termination cone discharging opening 4, cylinder 3 is connected with end cap 1 and/or discharging opening 4 removable seal.
The preferably a diameter of 50-200mm of cylinder 3, length is 200-1000mm.
Discharging opening 4 preferred length is 50-200mm, and outlet diameter is the 10-80% of cylinder 3 diameter, can be sparged into cylinder
Material in 3 forms whirlpool, plays well-mixed effect.
Nozzle 5 is gondola water faucet shape, spiral type or conical hollow, primarily serves the effect of dispersion feed liquid, can make participation reaction
Material contact area greatly increases, and mixing is more abundant；Using being detachably connected between nozzle 5 and feed pipe 2, conveniently will according to technique
Seek the nozzle changing multi-form, cleaning is also convenient.
Cylinder 3 inwall, equipped with least one flow-stopping plate 6, can further function as the effect increasing stirring, make mixed effect
More abundant.
During use, reactor is fixed in a certain splicing vessel port, each feed liquid pumps into from feed pipe 2 respectively, through nozzle 5
After dispersion or atomization, spurt in cylinder 3, after fast reaction or mixing, due to discharging opening 4 taper inhibition, in cylinder 3
Form whirlpool, then spray entrance splicing container from discharging opening 4, reaction completes.
It is only necessary to the outlet 4 of a reaction unit be connected to the feed pipe 2 of another reaction unit when being applied in combination
Some import, valve closing is passed through in other imports, you can completes the combination of reaction unit, is particularly suitable for stepwise reaction.
According to principles above, the invention still further relates to a kind of side preparing superfine rare-earth compound using reaction unit of the present invention
Method, can prepare superfine rare-earth compound.Rare earth feed liquid and precipitant press reaction ratio respectively from the different mouths of pipe of feed pipe 2
Enter, reacted postprecipitation slurry flows out from discharging opening (4), collect slurry, filter, wash, can get ultra-fine dilute after calcination
Earth compounds.
Rare earth feed liquid be lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, yttrium single or compound dilute
The solubility solution such as the hydrochlorate of earth elements, nitrate, sulfate or acetate, rare earth ion concentration is 0.1-2.0mol/l,
Feed temperature is 25-80 DEG C, and flow velocity is 0.2-6m3/h.
Precipitant is at least one of oxalic acid, Soluble oxalate salt, alkali carbonate, alkali metal hydroxide or ammonia
Solution, concentration be 0.1-6.0mol/l, temperature be 25-80 DEG C, flow velocity be 0.2-6m3/h.
Described rare earth feed liquid is re with the reaction molar ratio of precipitant3+: precipitant=1:(1.5-3.5).
Due to reaction unit small volume, when this device is used for precipitation, the material time of staying wherein is very short, sinks
Shallow lake granule has little time to grow up and is just ejected outside device, and high speed whirlpool can provide enough energy to grain crystalline again, thus heavy
Form sediment the grain graininess very little, distribution is also concentrated, and crystal formation is complete.D50≤1 μm can be prepared and be distributed the superfine rare-earth concentrated
Compound.
Advantages of the present invention:
1st, this reaction unit small volume, easy to use, and structure is simple, easily making, with low cost.
2nd, this reaction unit is detachable, changes part and cleaning is all very convenient, can single using it is also possible to 2 or many
Individual connection is applied in combination.
3rd, this reaction unit is applied to the mixing of fluid, dispersion, precipitation etc. some needs rapid-action field, either
Lab scale, pilot scale or industrialized production can use.
4th, it is prepared into granularity d50≤1 μm of superfine rare-earth compound using present device, granularity is little, distribution is concentrated, stream
Dynamic property is good.
Brief description
Fig. 1 is a kind of present invention reaction unit structural representation.
Fig. 2 is a kind of reaction unit structural representation equipped with flow-stopping plate for the present invention.
Fig. 3 is a kind of reaction unit structural representation of cross-feed mouth of the present invention..
In figure: 1- end cap, 2- feed pipe, 3- cylinder, 4- discharging opening, 5- nozzle, 6- flow-stopping plate
Specific embodiment
For the clearer description present invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
As shown in Figure 1, be the present invention a kind of reaction unit, including end cap 1, feed pipe 2, cylinder 3, discharging opening 4 and
Nozzle 5；Described feed pipe 2 is 2, stretches in cylinder 3 through end cap 1, the outlet ends of each feed pipe 2 are equipped with nozzle 5, cylinder
3 one end are connected with end cap 1, another termination cone discharging opening 4, and cylinder 3 is silk mouth with end cap 1 and discharging opening 4 and is connected.
According to technique needs, cylinder 3 intended diameter is 50mm, and length is 1000mm；Discharging opening 4 length is 50mm, and it goes out
The a diameter of 5mm of mouth；Nozzle 5 adopts spiral type, and silk mouth connects, and it is respond well that this device is used for emulsion reaction.
Embodiment 2
As shown in Figure 1, be the present invention a kind of reaction unit, including end cap 1, feed pipe 2, cylinder 3, discharging opening 4 and
Nozzle 5；Described feed pipe 2 is 2, stretches in cylinder 3 through end cap 1, the outlet ends of each feed pipe 2 are equipped with nozzle 5, cylinder
3 one end are connected with end cap 1, another termination cone discharging opening 4, and cylinder 3 is flange with end cap 1 and discharging opening 4 and is connected.
According to technique needs, cylinder 3 intended diameter is 200mm, and length is 200mm；Discharging opening 4 length is 200mm, and it goes out
The a diameter of 160mm of mouth；Nozzle 5 adopts gondola water faucet shape, silk mouth, this device is used for rare earth compound precipitation, can prepare grain
The rare earth compound of degree d50≤1 μm.
Embodiment 3
As shown in Figure 3, be the present invention a kind of reaction unit, including end cap 1, feed pipe 2, cylinder 3, discharging opening 4 and
Nozzle 5；Described feed pipe 2 is 3, and wherein 2 feed pipes 2 stretch in cylinder 3 through end cap 1, and another feed pipe 2 passes through circle
The wall of cylinder 3 stretches in cylinder 3, and equipped with nozzle 5, cylinder 3 one end is connected the outlet ends of each feed pipe 2 with end cap 1, another termination
Conical discharging opening 4, cylinder 3 is cutting ferrule with end cap 1 and discharging opening 4 and is connected.
According to technique needs, cylinder 3 intended diameter is 100mm, and length is 500mm；Discharging opening 4 length is 100mm, and it goes out
The a diameter of 50mm of mouth；Nozzle 5 adopts conical hollow, and cutting ferrule connects, and this device is used for the mixed of sulfonated kerosene and rare-earth extractant
Close, effect is very good.
Embodiment 4
As shown in Figure 2, be the present invention a kind of reaction unit, including end cap 1, feed pipe 2, cylinder 3, discharging opening 4 and
Nozzle 5；Described feed pipe 2 be 2, just stretch in cylinder 3 through end cap 1, the outlet ends of each feed pipe 2 equipped with nozzle 5,
Cylinder 3 one end is connected with end cap 1, another termination cone discharging opening 4, and cylinder 3 is silk mouth with end cap 1 and discharging opening 4 and is connected,
It is provided with 4 flow-stopping plates 6 in cylinder 3, bilayer is uniformly distributed.
According to technique needs, cylinder 3 intended diameter is 150mm, and length is 800mm；Discharging opening 4 length is 200mm, and it goes out
The a diameter of 100mm of mouth；Nozzle 5 adopts spiral type, and cutting ferrule connects, and this device can be used for mixing or the emulsifying of liquid.
Embodiment 5
Using the reaction unit of 2 embodiments 3, the outlet of one of reaction unit connects entering of another reaction unit
One of expects pipe, that is, complete the combination of 2 devices, and this combination unit can be used for two-step reaction or mixing.
Embodiment 6
Embodiment 2 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is Yttrium chloride(Y2Cl6), concentration is
0.5mol/l, temperature 60 C, flow rate set is 6m3/h；Precipitant is oxalic acid, and concentration is 1.0mol/l, 40 DEG C of temperature, and flow velocity sets
It is set to 6m3/ h, reaction molar ratio is re3+: oxalic acid=1:1.5, after end cap is arranged on filter tank, feed liquid and precipitant divide
Do not pump into from two mouths of pipe of feed pipe 2, after reacting in device, precipitate slurry flows out to filter tank from outlet 4, washing,
Filter, calcination obtains final product ultrafine yttria, detection granularity d10 is 0.31 μm, and d50 is 0.99 μm, and d90 is 2.96 μm.
Embodiment 7
Embodiment 3 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is Terbium nitrate (Tb(NO3)3), concentration is
2.0mol/l, temperature 50 C, flow rate set is 0.2m3/h；Precipitant is sodium carbonate, and concentration is 3.5mol/l, temperature 70 C, stream
Speed is set as 0.2m3/ h, reaction molar ratio is re3+: sodium carbonate=1:2, after end cap is arranged on reactor mouth, feed liquid and
Precipitant pumps into from the two of feed pipe 2 mouths of pipe respectively, and after reacting in device, precipitate slurry flows out to reactor from outlet 4
In, after ageing, blowing, to filter wash equipment, washs, and filters, and calcination obtains final product ultra-fine terbia. Diterbium trioxide, and detection granularity d10 is 0.32 μm, d50
For 0.92 μm, d90 is 3.12 μm.
Embodiment 8
Embodiment 3 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is cerous sulfate, concentration is
1.0mol/l, 25 DEG C of temperature, flow rate set is 3.0m3/h；Precipitant is ammonia, and concentration is 6mol/l, 25 DEG C of temperature, and flow velocity sets
It is set to 0.5m3/ h, reaction molar ratio is re3+: precipitant=1:3.5, after end cap is arranged on reactor mouth, feed liquid and heavy
Shallow lake agent pumps into from the two of feed pipe 2 mouths of pipe respectively, and after reacting in device, precipitate slurry flows out to reactor from outlet 4,
5 minutes blowings of ageing, to filter wash equipment, wash, filter, and calcination obtains final product fine cerium oxide, and detection granularity d10 is 0.31 μm, d50
For 0.98 μm, d90 is 3.37 μm.
Embodiment 9
Embodiment 2 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is lanthanum acetate, concentration is
0.1mol/l, 80 DEG C of temperature, flow rate set is 6.0m3/h；Precipitant is sodium hydroxide, and concentration is 0.1mol/l, 80 DEG C of temperature,
Flow rate set is 6m3/ h, reaction molar ratio is re3+: sodium hydroxide=1:3.0, after end cap is arranged on reactor mouth, material
Liquid and precipitant pump into from the two of feed pipe 2 mouths of pipe respectively, and after reacting in device, precipitate slurry flows out to anti-from outlet 4
Answer in kettle, 10 minutes blowings of ageing, to filter wash equipment, wash, filter, calcination obtains final product ultrafine lanthanum oxide, detection granularity d10 is
0.40 μm, d50 is 1.01 μm, and d90 is 3.10 μm.
Embodiment 10
Prepare superfine rare-earth compound using embodiment 2 device precipitation, rare earth feed liquid is lanthanum-cerium chloride terbium (55:30:15),
Concentration is 1.0mol/l, temperature 50 C, and flow rate set is 4.0m3/h；Precipitant is ammonium oxalate, and concentration is 0.5mol/l, temperature
60 DEG C, flow rate set is 6m3/ h, reaction molar ratio is re3+: precipitant=1:1.5, end cap is arranged on reactor mouth
Afterwards, feed liquid and precipitant pump into from the two of feed pipe 2 mouths of pipe respectively, and after reacting in device, precipitate slurry is from outlet 4 outflow
To in filter tank, washing, filter, calcination after centrifugation obtains final product ultrafine lanthanum oxide cerium terbium (55:30:15), and detection granularity d10 is 0.35
μm, d50 is 0.91 μm, and d90 is 3.01 μm.
Embodiment 11
Embodiment 4 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is lutecium chloride, concentration is
0.6mol/l, 30 DEG C of temperature, flow rate set is 2.0m3/h；Precipitant is oxalic acid: the mixture of Disodium oxalate .=1, oxalate concentration
For 1.0mol/l, 40 DEG C of temperature, flow rate set is 1.5m3/ h, reaction molar ratio is re3+: oxalate=1:2.0, by end cap
After being arranged on reactor mouth, feed liquid and precipitant pump into from the two of feed pipe 2 mouths of pipe respectively, after reacting, sink in device
Lodgment of stock material flows out to filter tank from outlet 4, washing, filters, and calcination after centrifugation obtains final product ultra-fine luteium oxide, and detection granularity d10 is
0.30 μm, d50 is 0.87 μm, and d90 is 2.77 μm.
Embodiment 12
Embodiment 3 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is Yttrium chloride(Y2Cl6) europium (5%eu),
Concentration is 1.mol/l, 40 DEG C of temperature, and flow rate set is 3.0m3/h；Precipitant is oxalic acid+ammonium oxalate (1+1), and concentration is
1.5mol/l, temperature 60 C, flow rate set is 3.0m3/ h, reaction molar ratio is re3+: precipitant=1:1.8, end cap is pacified
After being contained on reactor mouth, feed liquid and precipitant pump into from the two of feed pipe 2 mouths of pipe respectively, after reacting in device, precipitation
Slurry flows out to filter tank from outlet 4, washing, filters, and calcination obtains final product ultrafine yttria europium (5%eu), and detection granularity d10 is
0.4232 μm, d50 is 0.88 μm, and d90 is 3.02 μm.
Embodiment 13
Embodiment 3 device is utilized to prepare superfine rare-earth compound for precipitation, rare earth feed liquid is samarium trichloride, concentration is
0.8mol/l, temperature 50 C, flow rate set is 1.0m3/h；Precipitant is sodium bicarbonate, and concentration is 1.0mol/l, temperature 50 C,
Flow rate set is 3.0m3/ h, reaction molar ratio is re3+: precipitant=1:2.0, after end cap is arranged on reactor mouth, material
Liquid and precipitant pump into from the two of feed pipe 2 mouths of pipe respectively, and after reacting in device, precipitate slurry flows out to anti-from outlet 4
Answer in kettle, 15 minutes blowings of ageing, to filter wash equipment, wash, filter, be drying to obtain ultra-fine samaric carbonate, detection granularity d10 is
0.35 μm, d50 is 0.98 μm, and d90 is 3.63 μm.
Comparative example 1
Settling apparatus are reactor, and rare earth feed liquid is Yttrium chloride(Y2Cl6), and concentration is 0.5mol/l, 30 DEG C of temperature, and charging rate is
4m3/h；Precipitant is oxalic acid, and concentration is 0.5mol/l, 30 DEG C of temperature, and charging rate is 6m3/ h, reaction molar ratio is re3+:
Precipitant=1:1.5,150 revs/min of mixing speed, after having precipitated, washing, filter, calcination obtains yittrium oxide, detect granularity d10
For 0.62 μm, d50 is 2.65 μm, and d90 is 6.56 μm.
Finally illustrate, above example only in order to technical scheme to be described and unrestricted, although with reference to relatively
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, the objective without deviating from technical solution of the present invention and scope, and it all should be covered at this
In the middle of the right of invention.
Claims (10)
1. a kind of reaction unit is it is characterised in that include end cap (1), feed pipe (2), cylinder (3), discharging opening (4) and nozzle
(5)；Described feed pipe (2) at least 2, is respectively protruding in cylinder (3), the outlet ends of each feed pipe (2) are equipped with nozzle
(5), cylinder (3) one end is connected with end cap (1), the conical discharging opening (4) of another termination, cylinder (3) and end cap (1) and/or go out
Material mouth (4) connects for removable seal.
2. it is characterised in that a diameter of 50-200mm of described cylinder (3), length is reaction unit according to claim 1
200-1000mm.
3. reaction unit according to claim 1 and 2 it is characterised in that described discharging opening (4) length be 50-200mm,
Outlet diameter is the 10-80% of cylinder (3) diameter.
4. reaction unit according to claim 1 and 2 it is characterised in that described nozzle (5) be gondola water faucet shape, spiral type or
Conical hollow, is to be detachably connected with feed pipe (2).
5. according to claim 4 reaction unit it is characterised in that described cylinder (3) inwall is equipped with least one flow-stopping plate
(6).
6. a kind of prepare the method for superfine rare-earth compound it is characterised in that rare earth material using reaction unit described in claim 1
Liquid and precipitant are pressed reaction molar ratio and are entered from the different mouths of pipe of feed pipe (2) respectively, and reacted postprecipitation slurry is from discharging
Mouthful (4) flow out, and filter, washing, be dried or calcination after obtain final product superfine rare-earth compound.
7. prepare the method for superfine rare-earth compound according to claim 6 it is characterised in that described rare earth feed liquid be lanthanum,
Cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium, the hydrochlorate of single or compound rare-earth element of yttrium, nitrate,
Sulfate or acetate solution, concentration is 0.1-2.0mol/l, and temperature is 25-80 DEG C, and charging rate is 0.2-6m3/h.
8. prepare the method for superfine rare-earth compound according to claim 6 it is characterised in that described precipitant be oxalic acid,
At least one solution in Soluble oxalate salt, alkali carbonate, alkali metal hydroxide or ammonia, concentration is 0.1-
3.0mol/l, temperature is 25-80 DEG C, and charging rate is 0.2-6m3/h.
9. prepare the method for superfine rare-earth compound according to claim 6 it is characterised in that described rare earth feed liquid and precipitation
The reaction ratio of agent is re3+: precipitant=1:(1.5-3.5).
10. prepare the method for superfine rare-earth compound according to claim 6 it is characterised in that described superfine rare-earth chemical combination
Granularity d50≤1 μm of thing.
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