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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- 239000000843 powder Substances 0.000 title claims abstract description 70
- 238000005498 polishing Methods 0.000 title claims abstract description 67
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 64
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- FBJWDMHTMDVMIZ-UHFFFAOYSA-H C(C(=O)[O-])(=O)[O-].[Ce+3].[La+3].C(C(=O)[O-])(=O)[O-].C(C(=O)[O-])(=O)[O-] Chemical compound C(C(=O)[O-])(=O)[O-].[Ce+3].[La+3].C(C(=O)[O-])(=O)[O-].C(C(=O)[O-])(=O)[O-] FBJWDMHTMDVMIZ-UHFFFAOYSA-H 0.000 claims abstract description 48
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000004576 sand Substances 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 28
- 239000002699 waste material Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 23
- 238000000227 grinding Methods 0.000 claims description 14
- LEDZTLLWGZWUMH-UHFFFAOYSA-H cerium(3+) lanthanum(3+) trisulfate Chemical compound S(=O)(=O)([O-])[O-].[Ce+3].[La+3].S(=O)(=O)([O-])[O-].S(=O)(=O)([O-])[O-] LEDZTLLWGZWUMH-UHFFFAOYSA-H 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 235000006408 oxalic acid Nutrition 0.000 claims description 9
- 206010013786 Dry skin Diseases 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- -1 sulfuric acid rare earth salt Chemical class 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 230000008030 elimination Effects 0.000 claims description 2
- 238000003379 elimination reaction Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000001238 wet grinding Methods 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000005304 optical glass Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 3
- 229910052912 lithium silicate Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000713 high-energy ball milling Methods 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
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- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000003978 infusion fluid Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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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| CN103059737A (en) * | 2013-01-25 | 2013-04-24 | 湖南皓志新材料股份有限公司 | Preparation method of rare earth polishing powder with high polishing rate |
| 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 | A kind of equipment and method for preparing carbon black by plasma countercurrent cracking of gaseous hydrocarbons |
| 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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| JPH05147931A (en) * | 1991-11-25 | 1993-06-15 | Shin Etsu Chem Co Ltd | Production of oxide of rare earth element |
| JPH08267355A (en) * | 1995-04-03 | 1996-10-15 | Fujimi Inkooporeetetsudo:Kk | Manufacture of abrasive fine powder |
| 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 |
| CN101550318B (en) * | 2008-04-03 | 2012-11-14 | 北京有色金属研究总院 | Ce3+ -contained rare-earth polishing powder and preparation method thereof |
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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. |