CN102925106A - Rare earth polishing powder and preparation method thereof - Google Patents
Rare earth polishing powder and preparation method thereof Download PDFInfo
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- CN102925106A CN102925106A CN2012104551413A CN201210455141A CN102925106A CN 102925106 A CN102925106 A CN 102925106A CN 2012104551413 A CN2012104551413 A CN 2012104551413A CN 201210455141 A CN201210455141 A CN 201210455141A CN 102925106 A CN102925106 A CN 102925106A
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Abstract
The invention discloses a preparation method of white rare earth. Precipitant is added into soluble cerium-rich mixed rare earth salt solution to obtain mixed rare earth precipitate. Partial mixed rare earth precipitate is taken to completely react with fluridizer so that rare earth fluoride is obtained. The rare earth fluoride is mixed with residual mixed rare earth after preliminary roasting, and at last the polishing powder with high quality and high performance is produced after wet grinding, drying, smashing, filtering and roasting. The prepared polishing powder has the advantages of being small in median particle diameter and narrow in size distribution, D 50 <=2.5 micrometers, and the quality of products is stable.
Description
Technical field
The present invention relates to a kind of polishing powder from rare earth and preparation method thereof, particularly relate to the preparation method that polishing powder is used in a kind of liquid-crystal display polishing.
Background technology
Polishing powder from rare earth has the advantages that as a kind of good abrasive substance polishing velocity is fast, precision is high.
It is raw material that early stage polishing powder adopts hamartite, develops into afterwards take mixed rare earth carbonate as the raw material production polishing powder.Its production method has: a kind of is by mixed rare earth carbonate being carried out fluoridation, through roasting, airflow crash, classification, making product.Another kind of production method is first mixed chlorinated rare earth to be added silicofluoric acid to fluoridize, and obtains mixed rare earth carbonate by ammonium bicarbonate precipitation again, and high-temperature roasting, airflow crash, classification make finished product.But these two kinds of modes of fluoridizing have certain shortcoming, adopt the technique of fluoridizing behind the first ammonium bicarbonate precipitation, after high-temperature roasting, firmly and larger rare earth fluorine particle appears easily, separated in final progressive operation, cause product fluorine content unstable, thereby quality product easily fluctuate and affect the quality of product; And adopt fluoridize first after the technique of ammonium bicarbonate precipitation again, after fluoridizing, form unbodied rare earth fluorine floss precipitation, be difficult to carry out solid-liquid separation.
Therefore, need a kind of new polishing powder production technique of exploitation.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, and a kind of polishing powder from rare earth and preparation method thereof is provided, and it adopts the new mode of fluoridizing, thereby makes the content of fluorine more even, obtains little, the narrow particle size distribution of product granularity, its D
50The white polishing powder of≤2.5 μ m.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of polishing powder from rare earth, in polishing powder from rare earth, the proportion by weight of each rare earth oxide is: CeO
2Be 65～80 parts, La
2O
3Be 19～35 parts, Pr
6O
11＜=1 part, Nd
2O
3＜=1 part; The proportion by weight of fluorine is 1～10 part.
The present invention provides a kind of preparation method of described polishing powder from rare earth simultaneously, and described preparation method comprises the steps:
1), precipitation: with CeO
2Be 65～80 parts, La
2O
3Be 19～35 parts, Pr
6O
11＜=1 part, Nd
2O
3＜=1 part mishmetal salts solution and precipitation agent form the mishmetal precipitation 20～80 ℃ of reactions;
2), fluoridize: will account for the mishmetal precipitation of mishmetal precipitation total mass 8 ~ 22%, after adding water and sizing mixing with fluorizating agent 20～80 ℃ of complete reactions, the formation rare earth fluoride;
3), preroasting, rare earth fluoride is at 200～500 ℃ of preroasting 3～10h;
4), wet ball mill: rare earth fluoride and remainder mishmetal precipitation is mixed, size mixing, ball milling, sieve;
5), dry, pulverize, sieve: the mixture behind the wet ball mill is dried, pulverizes, sieved, obtain the precursor of polishing powder;
6), roasting: the precursor of polishing powder at 650 ℃～1100 ℃ lower roasting 3h～10h, is obtained polishing powder.
Described mishmetal salts solution is rare earth chloride, rare earth nitrate or their mixing salt solution; Its rare earth concentration (REO) is 30～150g/l, and 20～80 ℃ of lower preheatings.
Described precipitation agent is one or both and the above mixture in bicarbonate of ammonia, volatile salt, oxalic acid, the ammoniacal liquor.
The precipitation agent concentration of precipitin reaction is 0.5～1.8mol/l, and 20～80 ℃ of lower preheatings, adds precipitation agent and stops to add precipitation agent to pH=6.5, in 40～80 ℃ of lower ageing 0.5～10h, filtering separation.
Described fluorizating agent is hydrofluoric acid, Neutral ammonium fluoride or silicofluoric acid; The temperature of fluoridation is 20～70 ℃, to mishmetal precipitation perfluorination, filtering separation after the reaction.
In the described preroasting step, rare earth fluoride is at 200～500 ℃ of preroasting 3～10h.
Batch mixing after sieving after oven dry below 250 ℃, was pulverized 100～200 mesh sieves.
With the batch mixing after sieving at 800～1100 ℃ of lower roasting 2～8h,, make the polishing powder finished product.
In the finished product, the content of fluorine accounts for the polishing powder mass percent between 1～10%, and particularly preferred result is between 3～7%.
The white polishing powder from rare earth that the present invention produces, the content of fluorine is even, and product granularity is little, narrow particle size distribution, its D
50≤ 2.5 μ m.Use the result to show that it can satisfy requirement on industrial application, have high, the characteristics such as suspension is good, pH of suspension value stabilization, long service life of polishing qualification rate, this producing and manufacturing technique is stable, pollute little, raw material supply is abundant, and environmental benefit is good, is convenient to suitability for industrialized production, it is low to have production cost, powder characteristic be convenient to control, simple to operate, adapt to the advantages such as wide.
Description of drawings
Fig. 1 is the X diffraction spectrogram of the polishing powder of embodiment 1 preparation.
Fig. 2 is the particle size distribution figure of the polishing powder of embodiment 1 preparation.
Fig. 3 is the particle size distribution figure of the polishing powder of embodiment 2 preparations.
Embodiment
Get the lanthanum-cerium chloride solution 1000ml of 50g/l, CeO
-2/ TREO=66.4%, La
2O
3/ TREO=33.2% is in 50 ℃ of lower preheating 0.5h.Dropping stops during to pH=6.5 at the ammonium bicarbonate soln of the 0.9mol/l of 50 ℃ of preheating 0.5h, is stirred to react completely.In 40 ℃ of ageing 2h, filter, obtain mixed carbonic acid lanthanum cerium.
Mixed carbonic acid lanthanum cerium with 16.5% adds the size mixing HF(40% of rear adding 6ml of water) after 40 ℃ of lower reactions, filter, at 300 ℃ of preroasting 2.5h, obtain mixed fluoride lanthanum cerium.
With the mixed fluoride lanthanum cerium mixing of remaining mixed carbonic acid lanthanum cerium and preroasting, size mixing, filter behind the ball milling 1h, under 150 ℃, dry, pulverize, cross 200 mesh sieves, obtain the polishing powder precursor.
Precursor at 950 ℃ of lower calcining 5h, is namely obtained the polishing powder product.
Recording its specific surface area is 3.4850m
2/ g, D
50=2.24 μ m.
Fig. 1 is the X diffraction spectrogram of the polishing powder of embodiment 1 preparation.
Fig. 2 is the particle size distribution figure of the polishing powder of embodiment 1 preparation.
Get the lanthanum-cerium chloride solution 500ml of 100g/l, CeO
-2/ TREO=81.7%, La
2O
3/ TREO=18.2% is in 50 ℃ of lower preheating 0.5h.Dropping stops during to pH=6.5 at the ammonium bicarbonate soln of the 0.9mol/l of 50 ℃ of preheating 0.5h, is stirred to react completely.In 40 ℃ of ageing 2h, filter, obtain mixed carbonic acid lanthanum cerium.
Mixed carbonic acid lanthanum cerium with 14.3% adds the size mixing HF(40% of rear adding 5ml of water) after 40 ℃ of lower reactions, filter, at 300 ℃ of preroasting 2.5h, obtain mixed fluoride lanthanum cerium.
With mixed fluoride lanthanum cerium and the remaining mixed carbonic acid lanthanum cerium mixing of preroasting, size mixing, filter behind the ball milling 1h, under 150 ℃, dry, pulverize, cross 200 mesh sieves, obtain the polishing powder precursor.
Precursor at 1000 ℃ of lower calcining 4h, is namely obtained the polishing powder product.
Recording its specific surface area is 2.3183m
2/ g, D
50=1.26 μ m.
Fig. 3 is the particle size distribution figure of the polishing powder of embodiment 2 preparations.
It should be noted that at last: obviously, above-described embodiment only is for example of the present invention clearly is described, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here need not also can't give all embodiments exhaustive.And the apparent variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (9)
1. polishing powder from rare earth, it is characterized in that: in polishing powder from rare earth, the proportion by weight of each rare earth oxide is: CeO
2Be 65～80 parts, La
2O
3Be 19～35 parts, Pr
6O
11＜=1 part, Nd
2O
3＜=1 part; The proportion by weight of fluorine is 1～10 part.
2. the preparation method of polishing powder from rare earth as claimed in claim 1 is characterized in that, described preparation method comprises the steps:
1), precipitation: with CeO
2Be 65～80 parts, La
2O
3Be 19～35 parts, Pr
6O
11＜=1 part, Nd
2O
3＜=1 part mishmetal salts solution and precipitation agent form the mishmetal precipitation 20～80 ℃ of reactions;
2), fluoridize: will account for the mishmetal precipitation of mishmetal precipitation total mass 8 ~ 22%, after adding water and sizing mixing with fluorizating agent 20～80 ℃ of complete reactions, the formation rare earth fluoride;
3), preroasting, rare earth fluoride is at 200～500 ℃ of preroasting 3～10h;
4), wet ball mill: rare earth fluoride and remainder mishmetal precipitation is mixed, size mixing, ball milling, sieve;
5), dry, pulverize, sieve: the mixture behind the wet ball mill is dried, pulverizes, sieved, obtain the precursor of polishing powder;
6), roasting: the precursor of polishing powder at 650 ℃～1100 ℃ lower roasting 3h～10h, is obtained polishing powder.
3. the preparation method of polishing powder from rare earth as claimed in claim 2 is characterized in that, described mishmetal salts solution is rare earth chloride, rare earth nitrate or their mixing salt solution; Its rare earth concentration (REO) is 30～150g/l, and 20～80 ℃ of lower preheatings.
4. the preparation method of polishing powder from rare earth as claimed in claim 3 is characterized in that, described precipitation agent is one or both and the above mixture in bicarbonate of ammonia, volatile salt, oxalic acid, the ammoniacal liquor.
5. the preparation method of polishing powder from rare earth as claimed in claim 4 is characterized in that, the precipitation agent concentration of precipitin reaction is 0.5～1.8mol/l, and 20～80 ℃ of lower preheatings, add precipitation agent and stop to add precipitation agent to pH=6.5, in 40～80 ℃ of lower ageing 0.5～10h, filtering separation.
6. such as the preparation method of the described polishing powder from rare earth of claim 5, it is characterized in that described fluorizating agent is hydrofluoric acid, Neutral ammonium fluoride or silicofluoric acid; The temperature of fluoridation is 20～70 ℃, to mishmetal precipitation perfluorination, filtering separation after the reaction.
7. the preparation method of polishing powder from rare earth as claimed in claim 6 is characterized in that, in the described preroasting step, rare earth fluoride is at 200～500 ℃ of preroasting 3～10h.
8. the preparation method of polishing powder from rare earth as claimed in claim 7 is characterized in that, the batch mixing after sieving after oven dry below 250 ℃, was pulverized 100～200 mesh sieves.
9. the preparation method of polishing powder from rare earth as claimed in claim 8 is characterized in that, the batch mixing after sieving at 800～1100 ℃ of lower roasting 2～8h, is made the polishing powder finished product.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361030A (en) * | 2013-07-23 | 2013-10-23 | 内蒙古科技大学 | Praseodymium-containing ultrafine high-precision rare earth polishing powder and its preparation method |
| CN103468149A (en) * | 2013-09-18 | 2013-12-25 | 苏州市博飞光学有限公司 | Chlorinated rare earth polishing powder and production method thereof |
| CN104356947A (en) * | 2014-08-29 | 2015-02-18 | 海城海美抛光材料制造有限公司 | Two-stage intermediate preparation method for preparing rare earth polishing powders |
| CN105038604A (en) * | 2015-06-01 | 2015-11-11 | 华东理工大学 | Composition and preparation method of fluorine-containing rare-earth composite oxides |
| CN105505226A (en) * | 2015-12-02 | 2016-04-20 | 包头市新源抛光粉有限公司 | Rare earth polishing powder and preparation method thereof |
| CN106892572A (en) * | 2017-03-23 | 2017-06-27 | 宜昌南玻显示器件有限公司 | A kind of AG glass polishing solutions and AG process of glass |
| CN111115677A (en) * | 2020-01-13 | 2020-05-08 | 赣州有色冶金研究所 | Preparation method of rare earth fluoride |
| CN112357945A (en) * | 2020-11-06 | 2021-02-12 | 赣州湛海新材料科技有限公司 | Method for preparing high-purity yttrium oxyfluoride |
| CN113651352A (en) * | 2021-09-02 | 2021-11-16 | 甘肃稀土新材料股份有限公司 | Method for preparing low-calcium cerium lanthanum carbonate from high-calcium cerium lanthanum chloride solution |
| CN115286239A (en) * | 2022-08-04 | 2022-11-04 | 清远南玻节能新材料有限公司 | Glass, light scanning method thereof, cover plate and electronic equipment |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103361030A (en) * | 2013-07-23 | 2013-10-23 | 内蒙古科技大学 | Praseodymium-containing ultrafine high-precision rare earth polishing powder and its preparation method |
| CN103468149A (en) * | 2013-09-18 | 2013-12-25 | 苏州市博飞光学有限公司 | Chlorinated rare earth polishing powder and production method thereof |
| CN104356947A (en) * | 2014-08-29 | 2015-02-18 | 海城海美抛光材料制造有限公司 | Two-stage intermediate preparation method for preparing rare earth polishing powders |
| CN104356947B (en) * | 2014-08-29 | 2016-07-06 | 海城海美抛光材料制造有限公司 | Secondary intermediate is prepared method and is produced polishing powder from rare earth |
| CN105038604A (en) * | 2015-06-01 | 2015-11-11 | 华东理工大学 | Composition and preparation method of fluorine-containing rare-earth composite oxides |
| CN105505226A (en) * | 2015-12-02 | 2016-04-20 | 包头市新源抛光粉有限公司 | Rare earth polishing powder and preparation method thereof |
| CN106892572A (en) * | 2017-03-23 | 2017-06-27 | 宜昌南玻显示器件有限公司 | A kind of AG glass polishing solutions and AG process of glass |
| CN111115677A (en) * | 2020-01-13 | 2020-05-08 | 赣州有色冶金研究所 | Preparation method of rare earth fluoride |
| CN112357945A (en) * | 2020-11-06 | 2021-02-12 | 赣州湛海新材料科技有限公司 | Method for preparing high-purity yttrium oxyfluoride |
| CN112357945B (en) * | 2020-11-06 | 2023-12-08 | 赣州湛海新材料科技有限公司 | Method for preparing high-purity yttrium oxyfluoride |
| CN113651352A (en) * | 2021-09-02 | 2021-11-16 | 甘肃稀土新材料股份有限公司 | Method for preparing low-calcium cerium lanthanum carbonate from high-calcium cerium lanthanum chloride solution |
| CN115286239A (en) * | 2022-08-04 | 2022-11-04 | 清远南玻节能新材料有限公司 | Glass, light scanning method thereof, cover plate and electronic equipment |
| CN115286239B (en) * | 2022-08-04 | 2023-08-25 | 清远南玻节能新材料有限公司 | Glass, light sweeping method thereof, cover plate and electronic equipment |
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Application publication date: 20130213 |