CN102701259B - Preparation method of nano rare earth polishing powder - Google Patents
Preparation method of nano rare earth polishing powder Download PDFInfo
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- CN102701259B CN102701259B CN 201210155021 CN201210155021A CN102701259B CN 102701259 B CN102701259 B CN 102701259B CN 201210155021 CN201210155021 CN 201210155021 CN 201210155021 A CN201210155021 A CN 201210155021A CN 102701259 B CN102701259 B CN 102701259B
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Abstract
The invention relates to the technical field of material preparation, and specifically provides a method for preparing nano rare earth polishing powder with cerium lanthanum oxalate as a raw material. The method comprises the steps of: adding water to disperse cerium lanthanum oxalate serving as the raw material, carrying out wet grinding to average grain size smaller than 0.5mum with a nano sand mill, drying, carrying out high-temperature decomposition in a kiln to obtain rare earth oxide agglomerate powder, and crushing and dispersing the rare earth oxide agglomerate powder with an impact mill to obtain the nano rare earth polishing powder with the average grain size of 50-80nm. The prepared nano rare earth polishing powder has the characteristics of low process cost, high polishing efficiency and the like, and is particularly suitable for precision polishing of display screens of intelligent mobile telephones, optical glass and other products.
Description
Technical field
The present invention relates to technical field of material, a kind of preparation method of nano rare earth polishing powder further is provided.
Background technology
Physics, chemical property and good polishing performance that polishing powder from rare earth is unique with it, be widely used in the precise polished of the glass devices such as display screen glass, opticglass, ornaments and precision instrument.Along with increase and the national protective mining to the rare earth Mineral resources of polishing powder from rare earth consumption, polishing powder from rare earth is becoming tight supply day on the one hand; On the other hand, the polishing powder from rare earth waste residue formed in the polishing powder from rare earth use procedure is also in continuous increase.
In order to make valuable rare earth resources obtain more scientific rational utilization, should improve on the one hand polishing efficiency and the utilization ratio of polishing powder from rare earth; Regeneration and the recycle that realizes polishing powder from rare earth waste residue middle-weight rare earths composition on the other hand.
Aspect the polishing efficiency that improves polishing powder from rare earth, a very effective approach is to reduce the particle diameter of polishing powder from rare earth.Along with reducing of polishing powder from rare earth particle diameter, for the polishing powder of equal volume, when particle size is reduced to 0.1 micron from 1 micron, amounts of particles increases by 1000 times, and usually with a contact form, carry out micro-cutting processing between polishing powder and polished object body, thereby can significantly improve polishing efficiency.In addition, the polishing powder from rare earth that the cerium oxide of take is representative, except mechanical polishing, also can be realized chemical rightenning by the redoxomorphism of cerium ion.Along with the reduction of polishing powder particle diameter, specific surface area significantly increases, thereby the chemical rightenning effect is also significantly strengthened.
In the market the median size of polishing powder from rare earth generally between 0.5 ~ 2 micron, the part particle reaches 10 microns, polishing efficiency is not high, and the product ubiquity the shortcomings such as composition is unstable, granularity is inhomogeneous.At present, the above-mentioned shortcoming existed for domestic polishing powder from rare earth, a large amount of research has been done with regard to the preparation method of polishing powder from rare earth by some scientific research institutions, has also proposed some improvement projects.Scheme 1: a kind of production technique of superfine rare earth polishing powder, technical scheme: using cerous nitrate, praseodymium nitrate and organic solvent as raw material, then drip alkali lye, stirring and dissolving, obtain vitreosol; Again the vitreosol of gained is inserted in reacting kettle jacketing, carry out the water-bath evaporation, be converted into gel; The gel obtained is placed in to the drying receptacle inner drying, then the roasting insulation, monodispersed superfine rare earth polishing powder obtained.Scheme 2: rare earth ore concentrate prepares the method for high-cerium nano magnitude polishing powder from rare earth, technical scheme: production stage for directly making mixed rare earth carbonate from rare earth ore concentrate concentrated sulfuric acid roasting, infusion with ammonium bicarbonate precipitation method; Mixed rare earth carbonate mixes with alkali, is heated to 600-800 ℃, makes the mixture melting, and in molten state insulation 1-4 hour, cooling, as to pulverize, then add HF >=45% industrial hydrofluoric acid, the 10%-20% that its add-on is rare earth ore concentrate grain weight amount, obtain fluorine rare earth oxide enriched substance; By the rare enriched substance pulverizing of fluorine oxidation, washing, drainage, even in stirrer for mixing, then pack in band sieve high energy ball mill, be filled with nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber is with the high pressure draft rotating channel, and the lower powder of sieve, under the high velocity air promotion, dries processing to the moisture of powder, then dried.
Above method all has certain defect, has used fluorochemical, and environmental pollution is large, and the product cut size obtained is larger, and polishing efficiency is not high enough.Therefore, invent a kind of preparation method of nano rare earth polishing powder, to improving polishing efficiency and the utilization ratio of polishing powder from rare earth, save rare earth resources significant.
Summary of the invention
The technical problem to be solved in the present invention is, for the deficiencies in the prior art, the present invention aims to provide a kind of preparation method who does not need to use the nano rare earth polishing powder of the fluorochemicals such as hydrogen fluoride, thereby significantly improve polishing efficiency and the utilization ratio of polishing powder from rare earth, also be conducive to improve the surface brightness of polished goods simultaneously.
Technical scheme of the present invention is,
A kind of preparation method of nano rare earth polishing powder, concrete steps are:
(1) add deionized water in the lanthanum oxalate cerium and disperse, the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.2 ~ 2.0, obtains the dispersion liquid that contains the lanthanum oxalate cerium;
(2) with nanometer sand mill, the lanthanum oxalate cerium in dispersion liquid is ground to median size and is less than 0.5 micron, obtain the dispersion liquid after grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ ~ 120 ℃ dryings, in the lithium matter of then packing into crucible, in kiln under 800 ℃ ~ 1000 ℃ high temperature calcining and decomposing 1h ~ 6h, obtain rare earth oxide reunion powder;
(4) the rare earth oxide reunion powder that step (3) obtained disperses with impact grinding is broken, the nano rare earth polishing powder that to obtain average grain size be 50nm ~ 80nm.
Lanthanum oxalate cerium described in step (1) preferably reclaims the lanthanum oxalate cerium obtained from the polishing powder from rare earth waste residue, and in the lanthanum oxalate cerium, the atomic ratio of cerium and lanthanum is 1:0.1 ~ 0.5.
Described in step (3), kiln is selected from roller kiln, pushed bat kiln or drawer kiln.
Below the present invention is further explained and illustrates:
Equipment of the present invention is existing installation.
Nanometer sand mill in step (2) is to take zirconia ceramics as liner, the zirconia ceramics ball that the diameter of take is 0.5 ~ 1 millimeter is grinding medium, have mill and be situated between and automatically separate with material and the sand mill of material automated cycle grinding function, the grinding median size of material afterwards can be controlled between 0.3 ~ 0.5 micron.Preferred model is NT-X6L turbo-centrifugal nanometer sand mill.
In step (3), lithium matter crucible is a kind of crucible with very strong thermal shock resistance that approaches zero thermal expansion, and calcining can be roller kiln, pushed bat kiln or drawer kiln with kiln.
In step (4), impact grinding used is a kind of high-effect mill that is different from comminution by gas stream, and to be that rare earth oxide reunion powder that step (3) is obtained is broken disperse its Main Function, has that running noises is low, an automatic classification circulation, production efficiency high.
The lanthanum oxalate cerium is currently available products, can be commercial (as Chengdu four can rare earth Industrial Co., Ltd.s), also can from the polishing powder from rare earth waste residue, produce and obtain the lanthanum oxalate cerium, concrete steps following (detailed preparation process is shown in embodiment 1):
(1) the polishing powder from rare earth waste residue is carried out to physical separation, impurity elimination, and waste particle is crushed to below particle diameter 10mm, obtain the waste residue after broken;
(2) add the vitriol oil in the waste residue after step (1) fragmentation, control temperature of reaction at 120 ℃ ~ 180 ℃, react after 3 hours ~ 10 hours discharging while making material be cooled to below 100 ℃, obtain lanthanum sulfat cerium extract; The rare earth oxide content of the add-on of the vitriol oil in waste residue determine, 1.1 times ~ 1.5 times of theoretical requirement that all form sulfuric acid rare earth salt by rare earth oxide add the vitriol oil;
(3), by lanthanum sulfat cerium extract thin up and stir, then by the method for centrifugal or press filtration, lanthanum sulfat cerium extract is separated with solid residue;
(4) add oxalic acid in the lanthanum sulfat cerium extract separate obtained, obtain lanthanum oxalate cerium precipitation, it is terminal that the add-on of oxalic acid be take the white precipitate that the lanthanum oxalate cerium no longer occurs; Oxalic acid can be that the oxalic acid powder can be also oxalic acid aqueous solution, the oxalic acid aqueous solution that preferred mass concentration is 20%-30%;
(5) with centrifugal or filter-pressing method, lanthanum oxalate cerium throw out separated and wash to neutral, obtaining isolated waste liquid and lanthanum oxalate cerium throw out, lanthanum oxalate cerium throw out, 100 ℃ ~ 120 ℃ dryings, is obtained to lanthanum oxalate cerium finished product.
Compared with prior art, advantage of the present invention is:
(1) the present invention be take and produced the lanthanum oxalate cerium as raw material from the polishing powder from rare earth waste residue, makes the rare earth composition in the polishing powder from rare earth waste residue obtain efficient and high value added utilization, turns waste into wealth, and economizes on resources.
(2) technical process of the present invention is short, production efficiency is high, does not need to use the fluorochemicals, environmentally friendly such as hydrogen fluoride.
(3) the present invention can obtain the nano rare earth polishing powder that average grain size is 50nm ~ 80nm, and polishing rate is high.
The accompanying drawing explanation
fig. 1 is the transmission electron microscope photo of the nano rare earth polishing powder for preparing of the present invention, and its median size is 50nm ~ 80nm.
Embodiment
embodiment 1:
Reclaim from the polishing powder from rare earth waste residue and obtain the lanthanum oxalate cerium:
(1) get 1000 kilograms of rare earth polishing powder waste residues, after physical separation goes out obvious impurity, by its grain breakage to particle diameter 10mm;
(2) the polishing powder from rare earth waste residue after fragmentation is put in the glassed steel reaction vessels of 2500 liters, the vitriol oil that adds 900 kilogram 98%, use the heat-conducting oil heating reactor, 150 ℃ of lower impregnations 8 hours, discharging while then naturally cooling to below 100 ℃ in reactor, obtain lanthanum sulfat cerium extract;
(3) lanthanum sulfat cerium extract being diluted with water to total amount is 3000 liters, stirs, and then with pressure filter, lanthanum sulfat cerium extract is separated with solid residue and use the deionized water wash solid residue 5 times;
(4) add the oxalic acid aqueous solution that mass concentration is 20% in the lanthanum sulfat cerium infusion solution separate obtained, obtain white lanthanum oxalate cerium precipitation, until finish while adding oxalic acid solution no longer obvious sediment to occur;
(5) with pressure filter, lanthanum oxalate cerium throw out is separated, and extremely neutral with deionized water wash, obtain lanthanum oxalate cerium finished product after 100 ~ 120 ℃ of dryings;
(6) add lime to be precipitated the acid waste liquid separated in step (5), until the pH value of waste liquid reaches at 6.5 o'clock, stop adding lime, obtain by product gypsum and clear water.
embodiment 2:
(1) in from the polishing powder from rare earth waste residue, reclaiming the lanthanum oxalate cerium obtained, (atomic ratio of cerium and lanthanum is 1:0.2) adds the deionized water dispersion, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.5, obtains the dispersion liquid that contains the lanthanum oxalate cerium;
(2) with nanometer sand mill, the lanthanum oxalate cerium in dispersion liquid is ground to median size and is less than 0.5 micron, obtain the dispersion liquid after grinding;
(3) dispersion liquid after step (2) is ground is 120 ℃ of dryings, and in the lithium silicate matter of then packing into crucible, in kiln, calcining 5 hours under 800 ℃ of high temperature, obtain rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) obtained disperses with impact grinding is broken, the nano rare earth polishing powder that to obtain average grain size be 50nm.
embodiment 3:
(1) in the lanthanum oxalate cerium, (atomic ratio of cerium and lanthanum is 1:0.3) adds the deionized water dispersion, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:2.0, obtains the dispersion liquid that contains the lanthanum oxalate cerium;
(2) with nanometer sand mill, the lanthanum oxalate cerium in dispersion liquid is ground to median size and is less than 0.5 micron, obtain the dispersion liquid after grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ of dryings, and in the lithium silicate matter of then packing into crucible, in kiln, calcining 2 hours under 1000 ℃ of high temperature, obtain rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) obtained disperses with impact grinding is broken, the nano rare earth polishing powder that to obtain average grain size be 80nm.
embodiment 4:
(1) in from the polishing powder from rare earth waste residue, reclaiming the lanthanum oxalate cerium obtained, (atomic ratio of cerium and lanthanum is 1:0.4) adds the deionized water dispersion, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.75; Obtain the dispersion liquid that contains the lanthanum oxalate cerium;
(2) with nanometer sand mill, the lanthanum oxalate cerium in dispersion liquid is ground to median size and is less than 0.5 micron, obtain the dispersion liquid after grinding;
(3) dispersion liquid after step (2) is ground is 110 ℃ of dryings, and in the lithium silicate matter of then packing into crucible, in kiln, calcining 3.5 hours under 900 ℃ of high temperature, obtain rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) obtained disperses with impact grinding is broken, the nano rare earth polishing powder that to obtain average grain size be 60nm.
Claims (4)
1. the preparation method of a nano rare earth polishing powder, concrete steps are:
(1) add deionized water in the lanthanum oxalate cerium and disperse, the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.2 ~ 2.0, obtains the dispersion liquid that contains the lanthanum oxalate cerium;
(2) with nanometer sand mill, the lanthanum oxalate cerium in dispersion liquid is ground to median size and is less than 0.5 micron, obtain the dispersion liquid after grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ ~ 120 ℃ dryings, in the lithium matter of then packing into crucible, in kiln under 800 ℃ ~ 1000 ℃ high temperature calcining and decomposing 1h ~ 6h, obtain rare earth oxide reunion powder;
(4) the rare earth oxide reunion powder that step (3) obtained disperses with impact grinding is broken, the nano rare earth polishing powder that to obtain average grain size be 50nm ~ 80nm.
2. the preparation method of nano rare earth polishing powder according to claim 1, it is characterized in that: described in step (3), kiln is selected from roller kiln, pushed bat kiln or drawer kiln.
3. the preparation method of nano rare earth polishing powder according to claim 1, it is characterized in that: lanthanum oxalate cerium described in step (1) is to reclaim the lanthanum oxalate cerium obtained from the polishing powder from rare earth waste residue, and in the lanthanum oxalate cerium, the atomic ratio of cerium and lanthanum is 1:0.1 ~ 0.5.
4. the preparation method of nano rare earth polishing powder according to claim 3, it is characterized in that: the described concrete steps that reclaim the lanthanum oxalate cerium obtained from the polishing powder from rare earth waste residue are:
(1) the polishing powder from rare earth waste residue is carried out to physical separation, impurity elimination, and waste particle is crushed to particle diameter below 10mm, obtain the waste residue after broken;
(2) add the vitriol oil in the waste residue after step (1) fragmentation, control temperature of reaction at 120 ℃ ~ 180 ℃, react after 3 hours ~ 10 hours discharging while making material be cooled to below 100 ℃, obtain lanthanum sulfat cerium extract; The rare earth oxide content of the add-on of the vitriol oil in waste residue determine, 1.1 times ~ 1.5 times of theoretical requirement that all form sulfuric acid rare earth salt by rare earth oxide add the vitriol oil;
(3), by lanthanum sulfat cerium extract thin up and stir, then by the method for centrifugal or press filtration, lanthanum sulfat cerium extract is separated with solid residue;
(4) add oxalic acid in the lanthanum sulfat cerium extract separate obtained, obtain lanthanum oxalate cerium precipitation, it is terminal that the add-on of oxalic acid be take the white precipitate that the lanthanum oxalate cerium no longer occurs;
(5) with centrifugal or filter-pressing method, lanthanum oxalate cerium throw out separated and wash to neutral, obtaining isolated waste liquid and lanthanum oxalate cerium throw out, lanthanum oxalate cerium throw out, 100 ℃ ~ 120 ℃ dryings, is obtained to lanthanum oxalate cerium finished product.
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| CN106006701B (en) * | 2016-05-19 | 2018-06-12 | 福建省长汀金龙稀土有限公司 | A kind of preparation method of micrometer-submicrometer grade RE oxide powder |
| CN110591418A (en) * | 2019-10-21 | 2019-12-20 | 中昊黑元化工研究设计院有限公司 | Equipment and method for preparing carbon black by plasma countercurrent cracking of gaseous hydrocarbon |
| CN115321578B (en) * | 2022-09-08 | 2023-09-19 | 内蒙古科技大学 | Nano sphere-like rare earth fluoride polishing powder and preparation method thereof |
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| CN101357776A (en) * | 2002-06-07 | 2009-02-04 | 昭和电工株式会社 | Process for recovering rare earth oxide from waste liquid containing rare earth element, and process for producing rare earth oxide using same |
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Effective date of registration: 20220120 Address after: 410100 No. 20, Lixiang West Road, Changsha Economic and Technological Development Zone, Hunan Province Patentee after: HUNAN FENGYUAN YESHINE KINGCO NEW ENERGY Co.,Ltd. Address before: 410205 room 613, entrepreneurship building, Hunan University Science Park, No. 186, Guyuan Road, Yuelu District, Changsha City, Hunan Province Patentee before: HUNAN HANLIN NEW MATERIALS Co.,Ltd. |