CN101306828A - Device and process for preparing rare-earth compound uniform micro powder - Google Patents
Device and process for preparing rare-earth compound uniform micro powder Download PDFInfo
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Abstract
The invention provides a device for preparing rare earth compound uniform micro powders and a process thereof. The device comprises a static mixing reactor, a uniform crystallization tank with a stirring paddle, a feed liquid storage tank, a precipitating agent storage tank, and a flow rate, temperature and rotation speed control system. The device is used for precipitation synthesis of a single or compound rare earth carbonate, rare earth oxide, rare earth hydroxide, rare earth fluoride, rare earth oxalate or rare earth phosphate as well as compounds of rare earth and other metal. The method comprises the steps of adding a rare earth feed liquid and a precipitating agent feed liquid into the static mixing reactor, completely mixing the feed liquid in the reactor to form slurry with a crystal nucleus; and feeding the slurry into the uniform crystallization tank to obtain an uniform rare earth compound precursor, filtering, washing, drying, and calcinating to obtain rare earth compound micro powders with uniform particle size distribution, wherein the particle size can be adjusted in a range of 0.3-10 mum, and the particle size distribution (D90-D10)/D50 is less than 2. The rare earth compound prepared using the inventive device and process has the advantages of uniform particle size, narrow particle size distribution, good crystallization degree, good stability and less agglomeration. The inventive process is simple and applicable to industrial production.
Description
Technical field
The present invention relates to a kind of technology for preparing the device of rare-earth compound uniform micro powder and utilize this device preparation rare-earth compound uniform micro powder.
Technical background
The formation of ultrafine powder particle comprises two processes, i.e. nucleation process and particle growth process.Expect that it separately is gordian technique that uniform powder body material makes these two processes.And in the synthetic field of rare earth compound, because chemical precipitation method has the advantages that technology is simple, can accurately control chemical constitution, and be widely adopted, and extend to rare earth oxide, preparation field that polishing powder from rare earth, rare-earth luminescent material, rare earth form sediment rare earth materials such as thing, rare earth catalyst material altogether.The synthesizer of precipitator method employing at present mainly is the mechanical stirring reactor.But stirred autoclave can not make the nucleation process of powder particle and process of growth well separate as unique equipment of precipitin reaction, and therefore the homogeneity of product that obtains is poor, indexs such as yield rate is low, granularity, specific surface are wide in range, and product stability is bad.
Occur various special reaction apparatuses and method for this reason and prepared high-quality product.Patent CN1116146A discloses a kind of method for preparing ultrafine particle under gravity field, utilize the hypergravity device to finish the chemical precipitation method reaction as enhanced reactor, the product size-grade distribution is narrow, granularity is tiny, but this device is because the moving parts complexity, the requirement of shelter height, and there is certain difficulty in intensification and temperature control, and some product is not easy serialization production.
Chinese patent ZL01127978 discloses liquid phase nano-powder and nanoparticle aggregation structure preparation methods, and this method can make the size of nanoparticle controlled, epigranular, good dispersity, output height, simple, the less energy consumption of technology.This method is output particle after nucleation, do not have enough growth times, makes the particle stability that makes poor, reunites easily.
Concerning the preparation powder body material, the nucleation process of particle and crystallization process are separated, preparing uniform superfine powdery material becomes everybody goal in research.Device and the preparation method who when the preparation powder body material these two processes is separated also do not occur at present.
Summary of the invention
The invention provides a kind of technology for preparing the device of rare-earth compound uniform micro powder and utilize this device preparation rare-earth compound uniform micro powder.Can prepare superfine rare earth compound powder.
A kind of device for preparing rare-earth compound uniform micro powder, this device is by static mixing reactor, even crystallization groove, rare earth feed liquid storage tank, precipitation agent feed liquid storage tank and the flow, temperature, the speed control system that have stirring arm constitute, batch reactor has two opening for feeds at least, be respectively opening for feed 1 and opening for feed 2, can guarantee that rare earth feed liquid and precipitation agent feed liquid enter reactor respectively.The present invention adopts pipeline to realize connecting, and feed liquid storage tank, pump, batch reactor opening for feed 1 is connected, and precipitation agent storage tank, pump, batch reactor opening for feed 2 are connected; The batch reactor outlet is connected with even crystallization groove; Adopt pump to carry out the conveying of rare earth feed liquid and precipitation agent, for guaranteeing accurate conveying, be equipped with flow control system, the batch reactor that static mixing reactor selects for use feed liquid to carry with the piston flow pipe method therein, the device of preparation rare-earth compound uniform micro powder of the present invention, (this reactor market is on sale for rare earth feed liquid storage tank wherein, precipitation agent storage tank, static mixture reactor, the available trade mark is the static mixing reactor of SK type) and evenly the crystallization groove all be equipped with heating or attemperator and temperature controlling system, temperature is controlled at 18-100 ℃.
The device of preparation rare-earth compound uniform micro powder of the present invention, its rare earth feed liquid storage tank, precipitation agent storage tank or static mixture reactor outer wall chuck adopt oil bath, water-bath, water vapour or fused salt heating medium to heat.
Adopt device of the present invention to prepare the sedimentary technology of rare earth compound, its processing step is:
1) rare earth feed liquid for preparing and precipitation agent are stored in respectively separately in the hopper, and to its heat tracing;
2) pump into simultaneously in the static mixing reactor by the flow velocity of determining, two bursts of feed liquids thorough mixing in the flow process in reactor at a certain temperature forms the slurry of band nucleus;
3) slurry enters even crystallization groove insulation ageing and obtains homogenizing compound presoma;
4) after filtration, washing, dry, rare earth compound micro mist that roasting obtains obtaining even particle size distribution, its median particle diameter is adjustable between 0.3um-10um, size-grade distribution is: (D
90-D
10)/D
50＜2.
A kind of technology for preparing rare-earth compound uniform micro powder, rare earth compound are complex chemical compound single or compound rare-earth carbonate, rare earth oxide, rare-earth oxalate, rare-earth hydroxide, RE phosphate, rare earth fluorine and rare earth and other metal.
The present invention prepares the rare earth feed liquid that utilizes in the technology of rare-earth compound uniform micro powder and is the soluble ree salt, comprises single or compound rare-earth nitrate, lanthanon acetate, rare earth chloride or rare earth sulfate.
The present invention prepares the technology of rare-earth compound uniform micro powder, and precipitation agent comprises one or more in bicarbonate of ammonia, yellow soda ash, sodium bicarbonate, ammoniacal liquor, sodium hydroxide, oxalic acid, ammonium oxalate, sodium oxalate, phosphoric acid, ammonium phosphate, ammonium hydrogen phosphate, sodium phosphate, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, hydrofluoric acid, Neutral ammonium fluoride, the Sodium Fluoride.
Patent of the present invention is applied to directly nucleation process fast with the static reaction device, can guarantee that nucleus is after moment generates, can hightail original reaction system, the even crystallization groove that enters the band stirring carries out nuclei growth, thereby can not disturb the generation of back nucleus, can effectively nucleation and nuclei growth process be separated.Device of the present invention is used for the precipitation of the complex chemical compound of carbonated rare earth, rare-earth hydroxide, rare earth fluorine, rare earth oxalate and rare-earth phosphorate and rare earth and other metals and synthesizes.Be configured the principal feature of this cover synthesizer by even crystallization groove with static mixer and band stirring:
1, the median particle of product mainly concentrates on submicron to the interval territory of micron, and particle size distribution is narrow, and particle size uniformity is good;
2, the crucial synthesising part of this equipment does not have moving parts, easy to maintenance;
3, equipment capacity height, the flow velocity that depends on feed liquid and the caliber of production capacity.
The rare earth compound that utilizes device of the present invention and preparation technology to prepare has uniform particles, narrow particle size distribution, and crystallization degree is good, good stability, it is few to reunite.Technology is also fairly simple, realizes industrialization easily.
Figure of description
Fig. 1 is equipment configuration figure of the present invention.
Among Fig. 1,1 is the rare earth feed liquid storage tank, and 2 is the precipitation agent storage tank, and 3 is feed pump, and 4 is the precipitation agent pump, and 5 is static mixing reactor, and 6 is even crystallization groove, and 7 is the postprocessing working procedures of presoma.
Embodiment
Embodiment given below just gives further the present invention and describes, and those skilled in the art is to modification that the present invention did and improve all in the protection domain of claim qualification of the present invention.
Under the room temperature, compound concentration is the re chloride of 0.5mol/L and each 50L of ammonium bicarbonate soln of 1.5mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, start volume pump, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1.5m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, behind the heated and stirred 2h, dope filtration, washing back direct roasting obtain RE oxide powder.Size-grade distribution sees Table 1.
Under the room temperature, compound concentration is the re chloride of 0.5mol/L and each 50L of sodium carbonate solution of 1.5mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 0.6m/s in reactor, and the slurries that contain that generate from reactor directly enter in the even crystallization groove of being with stirring, heated and stirred 2h, dope filtration, washing back direct roasting obtain RE oxide powder.Size-grade distribution sees Table 1.
Under the room temperature, compound concentration is the re chloride of 0.5mol/L and each 50L of sodium hydrogen carbonate solution of 1.5mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 3h, dope filtration, washing after drying roasting at low temperatures obtain the rare earth carbonate powder.Size-grade distribution sees Table 1.
Compound concentration is the re chloride of 0.25mol/L and each 50L of ammoniacal liquor of 0.8mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, be heated to 50 ℃, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, it is 120 ℃ that reactor heats temperature outward, the flow velocity of mixed solution is 3m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back convection drying, roasting obtains the rare-earth hydroxide powder at low temperatures.Size-grade distribution sees Table 1.
Under the room temperature, compound concentration is the re chloride of 0.5mol/L and each 50L of sodium hydroxide solution of 1.5mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, be heated to 95 ℃ respectively, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, it is 150 degree that reactor heats temperature outward, the flow velocity of mixed solution is 1.2m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 5h, dope filtration, washing back convection drying obtains rare-earth hydroxide 150 ℃ of following roastings.Size-grade distribution sees Table 1.
Under the room temperature, compound concentration is the rare earth sulfate solution of 0.3mol/L and each 100L of oxalic acid solution of 0.45mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 2 in reactor, the precipitation slurries that contain that generate from reactor directly enter the precipitation slurries that contain that generate and directly enter in the even crystallization groove that band stirs from reactor, filter, washing back direct roasting obtains RE oxide powder.Size-grade distribution sees Table 1.
Compound concentration is the rare earth nitrate solution of 0.5mol/L and each 100L of ammonium oxalate solution of 1.0mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, be heated to 70 ℃, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 2m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter the precipitation slurries that contain that generate and directly enter in the even crystallization groove that band stirs evenly crystallization 20min from reactor, after filtration, washing, the drying, obtain the rare-earth oxalate powder 150 ℃ of following roastings.Size-grade distribution sees Table 1.
Embodiment 8
Compound concentration is the re chloride of 0.5mol/L and the mixing solutions of zirconium nitrate respectively, 1.0mol/L each 100L of sodium oxalate solution, put into rare earth feed liquid storage tank and precipitation agent storage tank, be heated to 70 ℃, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 2m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter the precipitation slurries that contain that generate and directly enter crystallization 20min in the even crystallization groove that band stirs from reactor, filter, washing back direct roasting obtains the composite oxide powder of rare earth and zirconium.Size-grade distribution sees Table 1.
Embodiment 9
Compound concentration is the acetic acid earth solution of 1.0mol/L and each 50L of phosphoric acid of 1.05mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare-earth phosphorate.Size-grade distribution sees Table 1.
Embodiment 10
Compound concentration is the rare earth nitrate solution of 1.0mol/L and each 50L of ammonium phosphate of 1.2mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare-earth phosphorate.Size-grade distribution sees Table 1.
Embodiment 11
Compound concentration is the re chloride of 1.0mol/L and each 150L of ammonium hydrogen phosphate of 1.0mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start material pump and flow measurement device simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare-earth phosphorate.Size-grade distribution sees Table 1.
Embodiment 12
Compound concentration is the rare earth nitrate solution of 1.0mol/L and each 50L of sodium phosphate of 1.1mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1.8m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 10h, dope filtration, alcohol washing back direct roasting obtain rare-earth phosphorate.Size-grade distribution sees Table 1.
Embodiment 13
Compound concentration is the rare earth chloride of 1.5mol/L and the mixing solutions of calcium chloride, each 50L of sodium hydrogen phosphate of 1.6mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, 3h is stirred in heating, and dope filtration, washing back direct roasting obtain the mixture of rare-earth phosphorate and calcium phosphate.Size-grade distribution sees Table 1.
Embodiment 14
Compound concentration is the acetic acid earth solution of 0.3mol/L and each 50L of Sodium phosphate dibasic of 0.4mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare-earth phosphorate.Size-grade distribution sees Table 1.
Embodiment 15
Compound concentration is the acetic acid earth solution of 1.0mol/L and each 100L of hydrofluoric acid of 3.2mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 2.2m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting rare earth fluorine.Size-grade distribution sees Table 1.
Embodiment 16
Compound concentration is the acetic acid earth solution of 1.0mol/L and each 50L of Neutral ammonium fluoride of 3.0mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare earth fluorine.Size-grade distribution sees Table 1.
Embodiment 17
Compound concentration is the rare earth nitrate solution of 1.0mol/L and each 50L of Sodium Fluoride of 3.0mol/L respectively, put into rare earth feed liquid storage tank and precipitation agent storage tank, under the room temperature condition, start volume pump simultaneously, squeeze into simultaneously in the static chemical combination reactor by opening for feed 1 and 2, the flow velocity of mixed solution is 1m/s in reactor, and the precipitation slurries that contain that generate from reactor directly enter in the even crystallization groove of band stirring, heated and stirred 2h, dope filtration, alcohol washing back direct roasting obtain rare earth fluorine.Granularity and distribution thereof see Table 1.
Related washing, drying and sinter process condition among the foregoing description 1-17 is to adopt rare earth compound micro mist common process condition.
Table 1 granularity and distribution
| Name of product | D 10(um) | D 50(um) | D 90(um) | |
| |
Rare earth oxide | 0.798 | 1.222 | 3.090 |
| |
Rare earth oxide | 0.550 | 0.930 | 2.230 |
| |
Rare earth carbonate | 0.413 | 0.850 | 1.605 |
| |
Rare earth oxide | 0.556 | 1.123 | 2.467 |
| |
Rare-earth hydroxide | 0.278 | 0.520 | 1.267 |
| |
Rare earth oxide | 2.400 | 9.623 | 19.900 |
| |
Rare earth oxalate | 2.350 | 4.532 | 11.000 |
| Embodiment 8 | The composite oxides of rare earth and zirconium | 0.791 | 1.543 | 3.890 |
| Embodiment 9 | Rare-earth phosphorate | 0.345 | 0.703 | 1.521 |
| Embodiment 10 | Rare-earth phosphorate | 0.870 | 1.589 | 3.612 |
| Embodiment 12 | Rare-earth phosphorate | 1.233 | 3.230 | 6.509 |
| Embodiment 13 | The mixture of rare-earth phosphorate and calcium phosphate | 1.123 | 2.577 | 5.890 |
| Embodiment 14 | Rare-earth phosphorate | 1.277 | 4.994 | 9.980 |
| Embodiment 15 | Rare earth fluorine | 0.127 | 0.367 | 0.779 |
| Embodiment 16 | Rare earth fluorine | 0.231 | 0.710 | 1.569 |
| Embodiment 17 | Rare earth fluorine | 0.390 | 0.980 | 2.234 |
Claims (8)
1, a kind of device for preparing rare-earth compound uniform micro powder, it is characterized in that, this device is made of static mixing reactor, even crystallization groove, feed liquid storage tank, precipitation agent storage tank and the flow, temperature, the speed control system that have a stirring arm, batch reactor has two opening for feeds at least, be respectively opening for feed 1 and opening for feed 2, can guarantee that rare earth feed liquid and precipitation agent feed liquid enter reactor respectively, feed liquid storage tank, pump, batch reactor opening for feed 1 are connected, and precipitation agent storage tank, pump, batch reactor opening for feed 2 are connected; The batch reactor outlet is connected with even crystallization groove.
2, according to claim 1-kind prepare the device of rare-earth compound uniform micro powder, it is characterized in that, adopt pump to carry out the conveying of rare earth feed liquid and precipitation agent, for guaranteeing accurate conveying, be equipped with flow control system, the batch reactor that static mixing reactor selects for use feed liquid to carry with the piston flow pipe method therein.
3, according to a kind of device for preparing rare-earth compound uniform micro powder of claim 1, it is characterized in that, rare earth feed liquid storage tank, precipitation agent storage tank, static mixture reactor and even crystallization groove all are equipped with heating or attemperator and temperature controlling system, and temperature is controlled at 18-100 ℃.
According to a kind of device for preparing rare-earth compound uniform micro powder of claim 1, it is characterized in that 4, rare earth feed liquid storage tank, precipitation agent storage tank or static mixture reactor outer wall chuck adopt oil bath, water-bath, water vapour or fused salt heating medium to heat.
5, adopt the described device of claim 1 to prepare the technology of rare-earth compound uniform micro powder, its processing step is:
(1) rare earth feed liquid for preparing and precipitation agent are stored in respectively separately in the hopper, and to its heat tracing;
(2) pump into simultaneously in the static mixing reactor by the flow velocity of determining, two bursts of feed liquids thorough mixing in the flow process in reactor at a certain temperature forms the slurry of band nucleus;
(3) slurry enters even crystallization groove insulation ageing, obtains uniform rare earth compound presoma;
(4) the rare earth compound presoma after filtration, washing, dry, rare earth compound micro mist that roasting obtains even particle size distribution, its median particle diameter is adjustable between 0.3um-10um, size-grade distribution is: (D
90-D
10)/D
50＜2 rare earth compound.
6, according to a kind of technology for preparing rare-earth compound uniform micro powder of claim 5, it is characterized in that rare earth compound is a complex chemical compound single or compound rare-earth carbonate, rare earth oxide, rare-earth oxalate, rare-earth hydroxide, RE phosphate, rare earth fluorine and rare earth and other metal.
7, according to a kind of technology for preparing rare-earth compound uniform micro powder of claim 5, it is characterized in that rare earth feed liquid is the soluble ree salt, comprise single or compound rare-earth nitrate, lanthanon acetate, rare earth chloride or rare earth sulfate.
8, according to a kind of technology for preparing rare-earth compound uniform micro powder of claim 5, it is characterized in that precipitation agent comprises one or more in bicarbonate of ammonia, yellow soda ash, sodium bicarbonate, ammoniacal liquor, sodium hydroxide, oxalic acid, ammonium oxalate, sodium oxalate, phosphoric acid, ammonium phosphate, ammonium hydrogen phosphate, sodium phosphate, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, hydrofluoric acid, Neutral ammonium fluoride, the Sodium Fluoride.
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