CN102701259A - Preparation method of nano rare earth polishing powder - Google Patents
Preparation method of nano rare earth polishing powder Download PDFInfo
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- CN102701259A CN102701259A CN2012101550211A CN201210155021A CN102701259A CN 102701259 A CN102701259 A CN 102701259A CN 2012101550211 A CN2012101550211 A CN 2012101550211A CN 201210155021 A CN201210155021 A CN 201210155021A CN 102701259 A CN102701259 A CN 102701259A
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- lanthanum oxalate
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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
[0001] 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
Polishing powder from rare earth has been widely used in the precise polished of glass devices such as display screen glass, opticglass, ornaments and precision instrument with its unique physics, chemical property and good polishing performance.Along with the 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 that in the polishing powder from rare earth use, forms is also in continuous increase.
In order to make valuable rare earth resources obtain more scientific and reasonable utilization, should improve the polishing efficiency and the utilization ratio of polishing powder from rare earth on the one hand; Be 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; As far as the polishing powder of equal volume, when particle size when 1 micron is reduced to 0.1 micron, amounts of particles increases by 1000 times; And carry out micro-cutting processing with a contact form usually between polishing powder and the polished object body, thereby can significantly improve polishing efficiency.In addition, the polishing powder from rare earth that with the cerium oxide is representative also can be realized chemical rightenning through the redoxomorphism of cerium ion except that mechanical polishing.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 shortcomings such as composition is unstable, granularity is inhomogeneous.At present, to the above-mentioned shortcoming that domestic polishing powder from rare earth exists, 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: with cerous nitrate, praseodymium nitrate and organic solvent as raw material, dripping alkali liquid again, stirring and dissolving obtains vitreosol; Again the vitreosol of gained is inserted in the reacting kettle jacketing, carry out the water-bath evaporation, be converted into gel; The gel that obtains is placed the drying receptacle inner drying, and roasting insulation again obtains monodispersed superfine rare earth polishing powder.Scheme 2: rare earth ore concentrate prepares the method for high-cerium nano magnitude polishing powder from rare earth, technical scheme: production stage is for directly to make mixed rare earth carbonate with ammonium bicarbonate precipitation method from rare earth ore concentrate concentrated sulfuric acid roasting, infusion; Mixed rare earth carbonate mixes with alkali, is heated to 600-800 ℃, makes the mixture fusion; And in molten state insulation 1-4 hour; Cool off, pulverize, add then the industrial hydrofluoric acid of HF >=45%, its add-on is the 10%-20% of rare earth ore concentrate grain weight amount, obtains fluorine rare earth oxide enriched substance; With the rare enriched substance pulverizing of fluorine oxidation, washing, drainage, even in stirrer for mixing, pack into then in the band sieve high energy ball mill, charge into nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel, and undersized powder dries processing to the moisture of powder under high velocity air promotes, dry again.
Above method all has certain defective, has used fluorochemical, and environmental pollution is big, and the product cut size that obtains is bigger, and polishing efficiency is not high enough.Therefore, invent a kind of preparation method of nano rare earth polishing powder, to improving the polishing efficiency and the utilization ratio of polishing powder from rare earth, it is significant to practice thrift rare earth resources.
Summary of the invention
The technical problem that the present invention will solve is; Deficiency to prior art; The present invention aims to provide a kind of preparation method that need not use the nano rare earth polishing powder of fluorochemicals such as hydrogen fluoride; Thereby significantly improve the polishing efficiency and the utilization ratio of polishing powder from rare earth, also help improving simultaneously the surface brightness of polished goods.
Technical scheme of the present invention does,
A kind of preparation method of nano rare earth polishing powder, concrete steps are:
(1) in the lanthanum oxalate cerium, add deionized water and disperse, the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.2 ~ 2.0, obtains containing the dispersion liquid of lanthanum oxalate cerium;
(2) with nanometer sand mill the lanthanum oxalate cerium in the dispersion liquid is ground to median size less than 0.5 micron, the dispersion liquid after must grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ ~ 120 ℃ dryings, in the lithium matter of packing into the then crucible, in kiln under 800 ℃ ~ 1000 ℃ high temperature calcining and decomposing 1h ~ 6h, rare earth oxide reunion powder;
(4) the rare earth oxide reunion powder that step (3) is obtained disperses with impact grinding is broken, and getting average grain size is the nano rare earth polishing powder of 50nm ~ 80nm.
Lanthanum oxalate cerium described in the step (1) preferably reclaims the lanthanum oxalate cerium that obtains from the polishing powder from rare earth waste residue, the atomic ratio of cerium and lanthanum is 1:0.1 ~ 0.5 in the lanthanum oxalate cerium.
Kiln is selected from roller kiln, pushed bat kiln or drawer kiln described in the step (3).
Below the present invention is done further explanation and explanation:
Equipment according to the invention is existing installation.
Nanometer sand mill in the step (2) is to be liner with the zirconia ceramics; With diameter is that 0.5 ~ 1 millimeter zirconia ceramics ball is a grinding medium; Have mill and be situated between and separate automatically with material and the sand mill of material automated cycle grinding function, the median size of material can be controlled between 0.3 ~ 0.5 micron after the grinding.Preferred model is the centrifugal nanometer sand mill of NT-X6L turbine.
Lithium matter crucible is a kind of crucible with very strong thermal shock resistance near zero thermal expansion in the step (3), and calcining can be roller kiln, pushed bat kiln or drawer kiln with kiln.
Used impact grinding is a kind of high-effect mill that is different from comminution by gas stream in the step (4), and it mainly acts on is broken dispersion of rare earth oxide reunion powder that step (3) is obtained, and has characteristics such as low, the automatic classification cycle of running noises, production efficiency height.
The lanthanum oxalate cerium is a currently available products, can be commercial (can rare earth Industrial Co., Ltd.s) like Chengdu four, also can from the polishing powder from rare earth waste residue, produce and obtain the lanthanum oxalate cerium, concrete steps are (detailed preparation process is seen embodiment 1) as follows:
(1) the polishing powder from rare earth waste residue is carried out physical separation, impurity elimination, and waste particle is crushed to below the particle diameter 10mm, the waste residue after broken;
(2) add the vitriol oil in the waste residue after step (1) fragmentation, control reaction temperature is at 120 ℃ ~ 180 ℃, reacts the discharging when making material be cooled to below 100 ℃ after 10 hours of 3 h ~, lanthanum sulfat cerium extract; The add-on of the vitriol oil confirmed by the rare earth oxide content in the waste residue, all form by rare earth oxide sulfuric acid rare earth salt theoretical requirement 1.1 times ~ 1.5 extraordinarily go into the vitriol oil;
(3), with the method for centrifugal or press filtration lanthanum sulfat cerium extract is separated with solid residue then with lanthanum sulfat cerium extract thin up and stir;
(4) in separating the lanthanum sulfat cerium extract that obtains, add oxalic acid, obtain lanthanum oxalate cerium deposition, the add-on of oxalic acid is a terminal point with the white precipitate that the lanthanum oxalate cerium no longer occurs; Oxalic acid can be that the oxalic acid powder also can be an oxalic acid aqueous solution, and preferred mass concentration is the oxalic acid aqueous solution of 20%-30%;
(5) with centrifugal or press filtration method lanthanum oxalate cerium throw out is separated and washing to neutral, isolated waste liquid and lanthanum oxalate cerium throw out, lanthanum oxalate cerium throw out 100 ℃ ~ 120 ℃ dryings, is promptly obtained lanthanum oxalate cerium finished product.
Compared with prior art, advantage of the present invention is:
(1) the present invention is a raw material from the polishing powder from rare earth waste residue, to produce the lanthanum oxalate cerium, 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, need not use 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.
Description of drawings
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:
From the polishing powder from rare earth waste residue, reclaim and obtain the lanthanum oxalate cerium:
(1) get 1000 kilograms of rare earth polishing powder waste residues, after physical separation goes out obvious impurity, with its grain breakage to particle diameter 10mm;
(2) the polishing powder from rare earth waste residue after the fragmentation is put in 2500 liters the glassed steel reaction vessels; The vitriol oil that adds 900 kilogram 98%; Use the heat-conducting oil heating reaction kettle; Flood reaction 8 hours down at 150 ℃, discharging when in reaction kettle, naturally cooling to below 100 ℃ then gets lanthanum sulfat cerium extract;
(3) be 3000 liters with lanthanum sulfat cerium extract thin up to total amount, stir, with pressure filter lanthanum sulfat cerium extract is separated with solid residue then and with deionized water wash solid residue 5 times;
(4) in the lanthanum sulfat cerium infusion solution that separate to obtain, adding mass concentration is 20% oxalic acid aqueous solution, obtains the lanthanum oxalate cerium deposition of white, finishes when oxalic acid solution no longer obvious sediment occurs until adding;
(5) with pressure filter lanthanum oxalate cerium throw out is separated, and extremely neutral with deionized water wash, after 100 ~ 120 ℃ of dryings, promptly obtain lanthanum oxalate cerium finished product;
(6) isolating acid waste liquid in the step (5) is added lime and precipitate, reach at 6.5 o'clock up to the pH of waste liquid value and stop to add lime, obtain by product gypsum and clear water.
Embodiment 2:
(1) (atomic ratio of cerium and lanthanum is 1:0.2) adds the deionized water dispersion in the lanthanum oxalate cerium that from the polishing powder from rare earth waste residue, reclaims acquisition, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.5, obtains containing the dispersion liquid of lanthanum oxalate cerium;
(2) with nanometer sand mill the lanthanum oxalate cerium in the dispersion liquid is ground to median size less than 0.5 micron, the dispersion liquid after must grinding;
(3) dispersion liquid after step (2) is ground is 120 ℃ of dryings, and in the lithium silicate matter of packing into the then crucible, calcining 5 hours in 800 ℃ of high temperature under in kiln must rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) is obtained disperses with impact grinding is broken, and getting average grain size is the nano rare earth polishing powder of 50nm.
Embodiment 3:
(1) (atomic ratio of cerium and lanthanum is 1:0.3) adds the deionized water dispersion in the lanthanum oxalate cerium, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:2.0, obtains containing the dispersion liquid of lanthanum oxalate cerium;
(2) with nanometer sand mill the lanthanum oxalate cerium in the dispersion liquid is ground to median size less than 0.5 micron, the dispersion liquid after must grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ of dryings, and in the lithium silicate matter of packing into the then crucible, calcining 2 hours in 1000 ℃ of high temperature under in kiln must rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) is obtained disperses with impact grinding is broken, and getting average grain size is the nano rare earth polishing powder of 80nm.
Embodiment 4:
(1) (atomic ratio of cerium and lanthanum is 1:0.4) adds the deionized water dispersion in the lanthanum oxalate cerium that from the polishing powder from rare earth waste residue, reclaims acquisition, and the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.75; Obtain containing the dispersion liquid of lanthanum oxalate cerium;
(2) with nanometer sand mill the lanthanum oxalate cerium in the dispersion liquid is ground to median size less than 0.5 micron, the dispersion liquid after must grinding;
(3) dispersion liquid after step (2) is ground is 110 ℃ of dryings, and in the lithium silicate matter of packing into the then crucible, calcining 3.5 hours in 900 ℃ of high temperature under in kiln must rare earth oxide reunion powder.
(4) the rare earth oxide reunion powder that step (3) is obtained disperses with impact grinding is broken, and getting average grain size is the nano rare earth polishing powder of 60nm.
Claims (4)
1. the preparation method of a nano rare earth polishing powder, concrete steps are:
(1) in the lanthanum oxalate cerium, add deionized water and disperse, the mass ratio of lanthanum oxalate cerium and deionized water is 1:1.2 ~ 2.0, obtains containing the dispersion liquid of lanthanum oxalate cerium;
(2) with nanometer sand mill the lanthanum oxalate cerium in the dispersion liquid is ground to median size less than 0.5 micron, the dispersion liquid after must grinding;
(3) dispersion liquid after step (2) is ground is 100 ℃ ~ 120 ℃ dryings, in the lithium matter of packing into the then crucible, in kiln under 800 ℃ ~ 1000 ℃ high temperature calcining and decomposing 1h ~ 6h, rare earth oxide reunion powder;
(4) the rare earth oxide reunion powder that step (3) is obtained disperses with impact grinding is broken, and getting average grain size is the nano rare earth polishing powder of 50nm ~ 80nm.
2. according to the preparation method of the said nano rare earth polishing powder of claim 1, it is characterized in that:
Lanthanum oxalate cerium described in the step (1) is from the polishing powder from rare earth waste residue, to reclaim the lanthanum oxalate cerium that obtains, and the atomic ratio of cerium and lanthanum is 1:0.1 ~ 0.5 in the lanthanum oxalate cerium.
3. according to the preparation method of the said nano rare earth polishing powder of claim 2, it is characterized in that: the said concrete steps that from the polishing powder from rare earth waste residue, reclaim the lanthanum oxalate cerium that obtains are:
(1) the polishing powder from rare earth waste residue is carried out physical separation, impurity elimination, and waste particle is crushed to particle diameter below 10mm, the waste residue after broken;
(2) add the vitriol oil in the waste residue after step (1) fragmentation, control reaction temperature is at 120 ℃ ~ 180 ℃, reacts the discharging when making material be cooled to below 100 ℃ after 10 hours of 3 h ~, lanthanum sulfat cerium extract; The add-on of the vitriol oil confirmed by the rare earth oxide content in the waste residue, all form by rare earth oxide sulfuric acid rare earth salt theoretical requirement 1.1 times ~ 1.5 extraordinarily go into the vitriol oil;
(3), with the method for centrifugal or press filtration lanthanum sulfat cerium extract is separated with solid residue then with lanthanum sulfat cerium extract thin up and stir;
(4) in separating the lanthanum sulfat cerium extract that obtains, add oxalic acid, obtain lanthanum oxalate cerium deposition, the add-on of oxalic acid is a terminal point with the white precipitate that the lanthanum oxalate cerium no longer occurs;
(5) with centrifugal or press filtration method lanthanum oxalate cerium throw out is separated and washing to neutral, isolated waste liquid and lanthanum oxalate cerium throw out, lanthanum oxalate cerium throw out 100 ℃ ~ 120 ℃ dryings, is promptly obtained lanthanum oxalate cerium finished product.
4. according to the preparation method of the said nano rare earth polishing powder of claim 1, it is characterized in that:
Kiln is selected from roller kiln, pushed bat kiln or drawer kiln described in the step (3).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059737A (en) * | 2013-01-25 | 2013-04-24 | 湖南皓志新材料股份有限公司 | Preparation method of high-polishing-rate rare-earth polishing powder |
| CN106006701A (en) * | 2016-05-19 | 2016-10-12 | 福建省长汀金龙稀土有限公司 | Preparation method of micron-submicron-scale rare earth 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 |
| CN115321578A (en) * | 2022-09-08 | 2022-11-11 | 内蒙古科技大学 | Nano quasi-spherical 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 |
| CN101550318A (en) * | 2008-04-03 | 2009-10-07 | 北京有色金属研究总院 | Ce<3+>-contained rare-earth polishing powder and preparation method thereof |
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2012
- 2012-05-18 CN CN 201210155021 patent/CN102701259B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN101550318A (en) * | 2008-04-03 | 2009-10-07 | 北京有色金属研究总院 | Ce<3+>-contained rare-earth polishing powder and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103059737A (en) * | 2013-01-25 | 2013-04-24 | 湖南皓志新材料股份有限公司 | Preparation method of high-polishing-rate rare-earth polishing powder |
| CN106006701A (en) * | 2016-05-19 | 2016-10-12 | 福建省长汀金龙稀土有限公司 | Preparation method of micron-submicron-scale rare earth oxide powder |
| 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 |
| CN115321578A (en) * | 2022-09-08 | 2022-11-11 | 内蒙古科技大学 | Nano quasi-spherical rare earth fluoride polishing powder and preparation method thereof |
| 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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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. |
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