CN103288119A - Preparation method of rear-earth polishing powder - Google Patents
Preparation method of rear-earth polishing powder Download PDFInfo
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- CN103288119A CN103288119A CN2013102401420A CN201310240142A CN103288119A CN 103288119 A CN103288119 A CN 103288119A CN 2013102401420 A CN2013102401420 A CN 2013102401420A CN 201310240142 A CN201310240142 A CN 201310240142A CN 103288119 A CN103288119 A CN 103288119A
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- rare earth
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Abstract
The invention discloses a preparation method of rear-earth polishing powder. The preparation method comprises the following steps of: (1), mixing rare earth carbonate with water, and adding a mineralizer for ageing to obtain alkaline type rare earth carbonate slurry; (2), adding a hydrofluoric acid solution to the alkaline type rare earth carbonate slurry for stirring for 1 hour to 3 hours and dehydrating to obtain rear-earth carbonate; (3), roasting the rear-earth carbonate to obtain rear-earth oxyfluoride; and (4), crushing and classifying the rear-earth oxyfluoride to obtain rear-earth polishing powder. The preparation method of the rear-earth polishing powder disclosed by the invention can be used for obtaining polishing powder of a special crystal form, so that the dimension size and morphology uniformity of the polishing powder particles are ensured without generating free fluorine ions and fluoride that affect the polishing precision and the polishing speed, and therefore, the crystallization degree is high; moreover, the product polishing powder is good in wear resistance, quick in polishing speed and easily controllable in polishing precision. Besides, the product is good in uniformity, high in production efficiency, low in cost, free of pollution and suitable for surface polishing machining of electronic information industrial precise apparatuses including an integrated circuit, a panel display, optical glass and the like.
Description
Technical field
The present invention relates to a kind of preparation method of polishing powder from rare earth, particularly a kind of preparation method of polishing powder from rare earth of the surface finish that is applied to electronics and information industry accurate devices such as unicircuit, plane demonstration, opticglass.
Background technology
At present, various glass materials are widely used, and these materials all need be through necessary surface finish before being employed.The early stage main materials such as zirconium white, ferric oxide or silicon-dioxide that use polish various glass surfaces, in recent years, consider that from polishing efficiency and precision aspect rare earth oxide (particularly cerium oxide) is considered to be more suitable for surface finish in glass material for the polishing material of main component.
Fast development along with electronic information technology, the demand of glass baseplates such as lens, sheet glass, liquid-crystal display (LCD), glasses, optical element and stupalith increases greatly, precision and polishing speed for polishing material are also had higher requirement, this just impels manufacturer to improve constantly product specification, to adapt to the requirement of new technology product innovation, polishing powder from rare earth has become applied widely, consumption rare earth application product big, with high content of technology now.
It is raw material that early stage polishing powder from rare earth adopts hamartite, be that the patent of invention of CN101215446A discloses the method that a kind of rare earth ore concentrate prepares high cerium nanometer scale polishing powder from rare earth as patent publication No., from rare earth ore concentrate concentrated sulfuric acid roasting, infusion, directly make mixed rare earth carbonate with hydrogen-carbonate by the precipitator method; Mixed rare earth carbonate mixes with alkali, is heated to fusion, and is incubated 1-4 hour in molten state, cools off, pulverizes, adds industrial hydrofluoric acid then, obtains fluorine rare earth oxide enriched substance; The rare enriched substance of fluorine oxidation, pulverize 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, sieve powder down dries processing to the moisture of powder under the high velocity air promotion, dry again handle polishing powder from rare earth.
CN101899281A discloses a kind of polishing powder from rare earth and preparation method thereof.This invention polishing powder contains cerium oxide, lanthanum trioxide, Praseodymium trioxide, and its total amount of rare earth TERO is more than 90wt%.For guaranteeing necessary polishing speed, in the wet method synthesis procedure, allocate the fluorine element that chemically reacts into, and controlled beginning to take shape of product granularity, make 877-3 type polishing powder from rare earth.
More use in the market be the heavy back of first carbon flaorination process, namely add bicarbonate of ammonia earlier and precipitate, add hydrofluoric acid after the washing again and fluoridize.
Be the production method that the patent of invention of CN100497508C discloses a kind of high-cerium rare-earth polishing powder as patent publication No., add hydrofluoric acid behind the preparation Phosbloc cerium earlier and fluoridize that roasting gets high-cerium rare-earth polishing powder.
The polishing powder that adopts above-mentioned existing production technique to produce can be disposable fluoridizing owing to what adopt, therefore have the inhomogeneous or local situation of fluoridizing of fluoridation, can influence on the one hand the crystal phase structure of product after the roasting, the free state fluorion of polishing precision and the speed of can exerting an influence on the other hand, the agglomerating particles size and the intensity that form after the roasting also have very big difference, and mainly being size and agglomeration strength by the coacervate particle that forms behind the high temperature sintering, the polishing precision of polishing powder and polishing speed determined, can cause a series of problems like this, for example the glass surface in polishing produces cut or polishing speed reduction fast in the very short time, particularly when throwing the hard glass surface, it is fatal that polishing speed reduces rapidly; The fluorine carbonated rare earth granularity that obtains in the fluorination process is less simultaneously, and the dehydration difficulty has caused output lower.
The polishing powder product that just need pick out certain agglomeration strength, certain particle size in order to satisfy condition, and these characteristics are to be difficult to control, and complex manufacturing, cost increases and introduces foreign ion, causes quality fluctuation.
In addition, be that the patent of invention of CN101010402A discloses rare earth oxide is mixed with rare earth fluoride as patent publication No., prepare the method for polishing powder from rare earth through grinding, drying, roasting, classification.The rare earth fluoride particle is thinner, the aftertreatment technology complexity; Use the also more complicated of technology that is mixed of fluorochemical and oxide compound simultaneously; This method can produce the phenomenon of particle double sintering, and the part particle produces unusual growth through re-baking, forms local big particle, thereby cause scuffing in polishing process.
Therefore, need a kind of polishing powder from rare earth and preparation method thereof especially, to solve the above-mentioned existing problem that exists.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polishing powder from rare earth, overcome the problems referred to above that prior art exists.
Preparation method of the present invention comprises the steps:
(1) preparation of basic carbonate rare earth
Carbonated rare earth is mixed with water, add mineralizer then, at 60-90 ℃ of ageing 3～5h, get basic carbonate rare earth slurries;
Described carbonated rare earth is selected from a kind of in Phosbloc cerium or the carbonic acid La-Ce-Pr;
Total amount of rare earth REO with described carbonated rare earth is benchmark, and each massfraction content of forming is
Cerium oxide (CeO
2/ TREO) 62-66%;
Lanthanum trioxide (La
2O
3/ TREO) 34-38%;
Praseodymium trioxide (Pr
6O
11/ TREO) 0～6%;
According to the massfraction meter, carbonated rare earth accounts for the 30%-40% of the weight summation of carbonated rare earth and water.
Described mineralizer is selected from a kind of in sodium hydroxide or the potassium hydroxide;
The add-on of described mineralizer is 1～2kg mineralizer/ton carbonated rare earth.
(2) fluoridize: under agitation condition weight concentration 20% hydrofluoric acid solution is joined in the basic carbonate rare earth slurries, finish the back and continue to stir 1-3h, dehydration gets the fluorine carbonated rare earth;
The consumption of described dropping 20% hydrofluoric acid solution is 90-105kg/ ton carbonated rare earth.
Described dehydration is selected from ordinary methods such as centrifuge dehydration, plate press filtration, vacuum hydro-extraction
(3) roasting: the fluorine carbonated rare earth is carried out roasting, get the fluorine rare earth oxide;
The maturing temperature of described fluorine carbonated rare earth roasting is 850-940 ℃, and roasting time is 5-7h.
(4) pulverize: with the pulverizing of fluorine rare earth oxide, classification, D50 is 1.0-2.0um, gets polishing powder from rare earth;
The grinding mode that described fluorine rare earth oxide is pulverized is selected from fluidized bed airflow and pulverizes or mechanical disintegration; Described classification is selected from jet classifying or hydrocyclone classification etc.
Term " REO " refers to rare earth oxide (abbreviation of Rare Earth Oxide);
Term " TREO " refers to total amount of the rare earth oxide (abbreviation of Total Rare Earth Oxides)
Term " CeO
2/ TREO " refer to the ratio that cerium oxide accounts for total amount of the rare earth oxide;
The cumulative particle sizes percentile that term " D50 " refers to a sample reaches 50% o'clock corresponding particle diameter.To be particle diameter account for 50% greater than its particle to its physical significance, also accounts for 50% less than its particle.
Polishing powder from rare earth of the present invention and preparation method thereof, compare with present product, by the carbonated rare earth pre-treatment, obtain specific crystal formation, size and the pattern uniformity coefficient of particle have been guaranteed, and then make fluoridation evenly complete, free state fluorion and the fluorochemical of do not exert an influence polishing precision and speed, degree of crystallinity height; The wear resistance of product polishing powder is good, and polishing speed is fast, and the polishing precision is controlled easily; The homogeneity of product is good, the production efficiency height, and cost is low, pollution-free, is applicable to the surface finish processing of electronics and information industry accurate devices such as unicircuit, plane demonstration, opticglass, realizes purpose of the present invention.
Description of drawings
Fig. 1 is the XRD synoptic diagram of embodiment 1 gained mishmetal polishing powder.
Embodiment 1
In the carbonated rare earth, the mass ratio of each component is: total amount of rare earth REO is 45%; Cerium oxide content (CeO
2/ TREO) be 62%, lanthanum trioxide content (La
2O
3/ TREO) be 38%;
Above-mentioned 1000kg carbonated rare earth is mixed with 2000kg water, add 1kg sodium hydroxide, after fully stirring, be heated to 60 ℃, ageing 5h.The hydrofluoric acid 90kg that adds weight concentration 20% then, after continuing to stir 1h, centrifuge dehydration gets the fluorine carbonated rare earth;
The fluorine carbonated rare earth at 940 ℃ of roasting 5h, is got fluorine rare earth oxide polishing powder presoma, then through comminution by gas stream, jet classifying, get described polishing powder from rare earth.This polishing powder is through laser particle analyzer test result: D
50=1.01 μ m.Fig. 1 is the XRD of gained mishmetal polishing powder.
Embodiment 2
In the carbonated rare earth, the mass ratio of each component is:
Total amount of rare earth REO is 45%; Cerium oxide content (CeO
2/ TREO) be 66%, lanthanum trioxide content (La
2O
3/ TREO) be 34%;
Above-mentioned 1000kg carbonated rare earth is mixed with 2000kg water, add 1.5kg sodium hydroxide, after fully stirring, be heated to 80 ℃, ageing 4h.Slowly add 20% hydrofluoric acid 95kg then, after continuing to stir 2h, centrifuge dehydration gets the fluorine carbonated rare earth;
The fluorine carbonated rare earth at 900 ℃ of roasting 6h, is got fluorine rare earth oxide polishing powder presoma, then through comminution by gas stream, jet classifying, get described polishing powder from rare earth.This polishing powder is through laser particle analyzer test result: D
50=1.8 μ m.
Embodiment 3
In the carbonated rare earth, the mass ratio of each component is:
Total amount of rare earth REO is 45%; Cerium oxide (CeO
2/ TREO) be 62%, lanthanum trioxide content (La
2O
3/ TREO) be 32%, Praseodymium trioxide content (Pr
6O
11/ TREO) be 6%;
Above-mentioned 1000kg carbonated rare earth is mixed with 1500kg water, add 2kg sodium hydroxide, after fully stirring, be heated to 90 ℃, ageing 3h.Slowly add 20% hydrofluoric acid 105kg then, after continuing to stir 3h, centrifuge dehydration gets the fluorine carbonated rare earth;
The fluorine carbonated rare earth at 850 ℃ of roasting 7h, is got fluorine rare earth oxide polishing powder presoma, then through comminution by gas stream, jet classifying, get described polishing powder from rare earth.This polishing powder is through laser particle analyzer test result: D
50=1.2 μ m.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and the specification sheets is principle of the present invention; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in the claimed scope of the present invention.The protection domain that the present invention requires is defined by appending claims and equivalent thereof.
Claims (8)
1. the preparation method of polishing powder from rare earth is characterized in that, comprises the steps:
(1) carbonated rare earth is mixed with water, add mineralizer then, ageing gets basic carbonate rare earth slurries;
(2) hydrofluoric acid solution is joined in the basic carbonate rare earth slurries, stir 1-3h, dehydration gets the fluorine carbonated rare earth;
(3) the fluorine carbonated rare earth is carried out roasting, get the fluorine rare earth oxide;
(4) with the pulverizing of fluorine rare earth oxide, classification, get polishing powder from rare earth.
2. method according to claim 1 is characterized in that, carbonated rare earth is mixed with water, adds mineralizer then, at 60-90 ℃ of ageing 3～5h.
3. method according to claim 1 is characterized in that, described carbonated rare earth is selected from a kind of in Phosbloc cerium or the carbonic acid La-Ce-Pr.
4. method according to claim 1 is characterized in that, the hydrofluoric acid solution of weight concentration 20% joins in the basic carbonate rare earth slurries, and the consumption of hydrofluoric acid solution is 90-105kg/ ton carbonated rare earth.
5. method according to claim 1 is characterized in that, the maturing temperature of described fluorine carbonated rare earth roasting is 850-940 ℃, and roasting time is 5-7h.
6. method according to claim 1 is characterized in that, with the pulverizing of fluorine rare earth oxide, classification, D50 is 1.0-2.0um, gets polishing powder from rare earth.
7. method according to claim 1 is characterized in that, described mineralizer is selected from a kind of in sodium hydroxide or the potassium hydroxide; The add-on of described mineralizer is 1～2kg mineralizer/ton carbonated rare earth.
8. according to each described method of claim 1～7, it is characterized in that, is benchmark with the total amount of rare earth REO of described carbonated rare earth, and each massfraction content of forming is:
Cerium oxide (CeO
2/ TREO) 62-66%;
Lanthanum trioxide (La
2O
3/ TREO) 34-38%;
Praseodymium trioxide (Pr
6O
11/ TREO) 0～6%;
According to the massfraction meter, carbonated rare earth accounts for the 30%-40% of the weight summation of carbonated rare earth and water.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792269A (en) * | 2014-01-23 | 2014-05-14 | 包头华美稀土高科有限公司 | Analytical method for directly measuring fluorine ion content in carbonic acid rare earth by using fluorine ion electrode method |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
| CN113969108A (en) * | 2021-11-18 | 2022-01-25 | 东北大学 | Method for preparing polishing solution for optical glass by using cerium enrichment as raw material |
| CN114539928A (en) * | 2022-03-16 | 2022-05-27 | 深圳市瑞来稀土材料有限公司 | Rare earth polishing powder for optical glass polishing treatment and preparation method thereof |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
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| CN101475777A (en) * | 2008-11-07 | 2009-07-08 | 上海华明高纳稀土新材料有限公司 | High precision rare earth polishing powder and preparation thereof |
| CN101967005A (en) * | 2010-07-20 | 2011-02-09 | 包头市京瑞新材料有限公司 | Method for preparing neodymium praseodymium fluoride with large granules and large specific surface area |
| CN102965026A (en) * | 2012-11-12 | 2013-03-13 | 上海华明高纳稀土新材料有限公司 | Rare-earth polishing powder and preparation method thereof |
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| CN101967005A (en) * | 2010-07-20 | 2011-02-09 | 包头市京瑞新材料有限公司 | Method for preparing neodymium praseodymium fluoride with large granules and large specific surface area |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792269A (en) * | 2014-01-23 | 2014-05-14 | 包头华美稀土高科有限公司 | Analytical method for directly measuring fluorine ion content in carbonic acid rare earth by using fluorine ion electrode method |
| CN103792269B (en) * | 2014-01-23 | 2016-04-20 | 包头华美稀土高科有限公司 | Fluoride ion electrode method directly measures the analytical approach of content of fluoride ion in carbonated rare earth |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN106044829B (en) * | 2016-05-25 | 2018-03-23 | 南昌大学 | A kind of preparation method of white pure zirconia cerium |
| CN106044829B8 (en) * | 2016-05-25 | 2018-11-27 | 赣州湛海工贸有限公司 | A kind of preparation method of white pure zirconia cerium |
| CN112724839A (en) * | 2021-01-21 | 2021-04-30 | 包头华明高纳稀土新材料有限公司 | System and method for preparing rare earth polishing powder |
| CN113969108A (en) * | 2021-11-18 | 2022-01-25 | 东北大学 | Method for preparing polishing solution for optical glass by using cerium enrichment as raw material |
| CN114539928A (en) * | 2022-03-16 | 2022-05-27 | 深圳市瑞来稀土材料有限公司 | Rare earth polishing powder for optical glass polishing treatment and preparation method thereof |
| CN115678436A (en) * | 2022-11-04 | 2023-02-03 | 包头市科蒙新材料开发有限责任公司 | Preparation method of novel cerium-rich rare earth polishing powder |
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Application publication date: 20130911 |