CN1482195A - Preparation method of rare-earth polishing powder - Google Patents

Preparation method of rare-earth polishing powder Download PDF

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Publication number
CN1482195A
CN1482195A CNA03130446XA CN03130446A CN1482195A CN 1482195 A CN1482195 A CN 1482195A CN A03130446X A CNA03130446X A CN A03130446XA CN 03130446 A CN03130446 A CN 03130446A CN 1482195 A CN1482195 A CN 1482195A
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China
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rare earth
polishing powder
ceo
preparation
polishing
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CNA03130446XA
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CN1194060C (en
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刘占泉
王连源
王庆梅
石春祥
汪根时
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Nankai University
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Nankai University
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Publication of CN1194060C publication Critical patent/CN1194060C/en
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  • Glass Compositions (AREA)

Abstract

The polishing RE powder contains CeO2, La2O3, Pr6O11 and Nd2O3 as main components and Ce content of 75-85 %. Its preparation includes the following steps: dissolving waste polishing RE powder in acid while adding H2O2 in 30 %; regulating pH value with ammonia water to 5-6; adding H2O2 in 30 % and suspension of RE hydroxide at 30-80 deg.c for complete precipitation; water washing, drying and roasting at 300-1200 deg.c for 4 hr to prepare regenerated polishing RE powder with high Ce content. The present invention makes it possible to utilize polishing RE powder fully and can save resource and reduce environmental pollution.

Description

The preparation method of polishing powder from rare earth
Technical field
The present invention relates to the preparation method of polishing powder from rare earth.
Background technology
Rare earth oxide has purposes widely, and one of important use wherein is the high-efficiency high-quality polishing material as glass.In recent years, only domestic requirement is annual more than 1,500 tons, has produced thus a large amount of useless polishing powder from rare earth.
Polishing powder from rare earth is a kind of mixed light rare-earth oxide, and main component is CeO 2, La 2O 3, Pr 6O 11, Nd 2O 3Etc..The polishing performance of polishing powder and CeO 2Content is closely related.Commercially available polishing powder is pressed CeO 2Content is divided into two big classes, and a class is CeO 2〉=80%, another kind of is CeO 2≤ 50%, the relevant factory of China mostly uses about 50% powder at present, owing to use the back of losing efficacy to abandon as waste material, this had both caused the waste to rare earth resources, had polluted environment simultaneously again.
Have multiple from mixed rare-earth oxide the method for separating cerium, for example Chinese patent CN1047110A discloses " novel method of separating cerium dioxide from mishmetal ", its needs the special ozone generating-device of a cover, is restricted in the application.All similar patents are all to isolate CeO in addition 2Be purpose, remaining rare earth is not utilized.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of polishing powder from rare earth, technological operation of the present invention is simple, and is with low cost, can be CeO in the useless polishing powder 2≤ 50% brings up to CeO 2〉=80%, make useless polishing powder from rare earth obtain farthest utilizing again.Save resource, reduced environmental pollution, its society, remarkable in economical benefits, and obtain high CeO 2The polishing powder from rare earth of content has improved the class of polishing powder, and its polishing performance is good.
The preparation method of polishing powder from rare earth of the present invention, wherein main component contains CeO 2, La 2O 3, Pr 6O 11, Nd 2O 3, described polishing powder from rare earth contains cerium amount 75-85%, and it may further comprise the steps:
1) will give up polishing powder from rare earth at 60-80 ℃, stir lower acid adding to the trivalent rare earth oxide dissolution, not molten CeO 2Solid sinks to the bottom.
2) stirring is lower, adds 30% H 2O 2Make CeO 2Dissolving, it is orange red that solution is.
3) stir lower add ammoniacal liquor, NH 3: H 2O=1: 1, regulate PH=5-6, add 30% H 2O 2, 50-90 ℃ of lower heating 1 hour.
4) light rare earths oxyhydroxide or the Ce (OH) of adding 5-8% 4Suspension, 30-80 ℃, stirred 4-12 hour, make precipitation fully, isolate precipitation, through being washed to neutrality, drying and 300-1200 ℃ of warm roasting 4 hours, through grinding the cerium-rich rare earth oxide compound that sieve series gets 1-10 μ m fine powder, promptly get the regeneration polishing powder from rare earth of high cerium content.When raw material is that useless polishing powder from rare earth (generally contains CeO 245-50%), obtain the regenerated polishing powder from rare earth through processing and contain CeO 2Bring up to 75-85%.
Described acid is hydrochloric acid or rare nitric acid.
Described useless polishing powder from rare earth and H 2O 2Mass/volume be 1: 0.3-0.5.
H2O2 is as oxidant among the present invention, again as reducing agent, and H 2O 2In oxygen, its oxidation number can be-1,0 ,-2, in acid solution, CeO 2Strong oxidizer, H 2O 2Become reducing agent.
CeO 2Along with reaction, be dissolved in acid and become trivalent ion to enter acid feed liquid with other trivalent rare earths.Under alkali condition, because current potential:
E 0=+0.87V
E 0=-1.74VH 2O 2Become oxidant this moment, and cerium is oxidized in alkali lye, because Ce (OH) 4Solubility product is minimum, along with Ce 4+Generate, PH>2 namely generate Ce (OH) 4Complete to PH 5-6 precipitation.And other trivalent rare earths are wanted just large quantities of precipitations of PH>7.As for a small amount of trivalent rare earth, because of adsorption effect with Ce (OH) 4Precipitate and go out for one, remainder is stayed in the filtrate.When hydroxide filtered, other added rare-earth hydroxide suspension, in order to accelerated filtration.
The present invention can be CeO in the useless polishing powder 2≤ 50% brings up to CeO 2〉=80%, make useless polishing powder from rare earth obtain farthest utilizing again.Technological operation of the present invention is simple, and the resource of having saved with low cost reduces environmental pollution, its society, remarkable in economical benefits, and obtain high CeO 2The polishing powder from rare earth of content has improved the class of polishing powder, and its polishing performance is good.
Embodiment
Embodiment:
Get levigate useless polishing powder, rare earth consists of CeO 248.12%, La 2O 332.24%, Pr 6O 113.3%, Nd 2O 34.3% 40 grams place beaker, add 4N HNO 3200 milliliters of solution, 80 ℃ of lower half an hour, trivalent rare earth oxide dissolution, CeO of stirring 2Solid sinks to the bottom, and major part is not molten, and pass to solution bottom with pipe this moment, adds gradually 30%H 2O 216ml, CeO 2Dissolving, it is orange red that solution is, and continues to stir adding ammoniacal liquor, (NH again 3: H 2O=1: 1) regulate PH=5.5, be heated to 50 ℃ this moment, 1 hour, in this process, continues to add H 2O 216ml has a large amount of orange-yellow precipitations to produce, and then adds 2 gram Ce (OH) 4Suspension, this mixture is heated to 80 ℃ then, stirs 12 hours, is washed to precipitation neutral and filters, drying obtains hydroxide.950 ℃ of roastings 4 hours get cerium-rich rare earth oxide compound 29.6 grams of 3-9ml through the mill sieve series.Its rare earth consists of CeO 280.05%, La 2O 33.03%, Pr 6O 111.02%, Nd 2O 31.01%.Productive rate is 74%.Recording product must the polishing ability be 60.2 (being worn away amount of glass mg/10min).

Claims (3)

1. the preparation method of a polishing powder from rare earth, wherein main component contains CeO 2, La 2O 3, Pr 6O 11, Nd 2O 3, it is characterized in that described polishing powder from rare earth contains cerium amount 75-85%, it may further comprise the steps:
1) will give up polishing powder from rare earth at 60-80 ℃, stir lower acid adding to the trivalent rare earth oxide dissolution, not molten CeO 2Solid sinks to the bottom;
2) stirring is lower, adds 30% H 2O 2Make CeO 2Dissolving, it is orange red that solution is;
3) stir lower add ammoniacal liquor, NH 3: H 2O=1: 1, regulate PH=5-6, add 30% H 2O 2, 50-90 ℃ of lower heating 1 hour;
4) light rare earth hydroxide or the Ce (OH) of adding 5-8% 4Suspension, 30-80 ℃, stirred 4-12 hour, make precipitation fully, isolate precipitation, through being washed to neutrality, drying and 300-1200 ℃ of warm roasting 4 hours, getting the regeneration polishing powder from rare earth that namely gets high cerium content of 1-10 μ m through the mill sieve series.
2, the preparation method of polishing powder from rare earth according to claim 1 is characterized in that described acid is hydrochloric acid or rare nitric acid.
3, the preparation method of polishing powder from rare earth according to claim 1 is characterized in that described useless polishing powder from rare earth and H 2O 2Mass/volume be 1: 0.3-0.5.
CNB03130446XA 2003-07-24 2003-07-24 Preparation method of rare-earth polishing powder Expired - Fee Related CN1194060C (en)

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Application Number Priority Date Filing Date Title
CNB03130446XA CN1194060C (en) 2003-07-24 2003-07-24 Preparation method of rare-earth polishing powder

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CN1194060C CN1194060C (en) 2005-03-23

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101899281A (en) * 2009-05-25 2010-12-01 甘肃稀土新材料股份有限公司 Rare earth polishing powder and production method thereof
CN101899264A (en) * 2009-05-25 2010-12-01 甘肃稀土新材料股份有限公司 Rare earth polishing powder and preparation method thereof
CN102251117A (en) * 2011-06-17 2011-11-23 金华冠华水晶有限公司 Method for extracting rare earth component from crystal waste slag
CN102391833A (en) * 2011-09-08 2012-03-28 金华冠华水晶有限公司 Method for recycling and applying discarded rare earth polishing powder into crystal glass
CN101280175B (en) * 2006-04-07 2012-07-25 清美化学株式会社 Method for regenerating cerium-based abrasive
CN102886308A (en) * 2012-10-15 2013-01-23 内蒙古科技大学 Method for recycling waste rare-earth polishing powder
CN103079764A (en) * 2010-08-03 2013-05-01 Ranco株式会社 Method for regenerating ceria-based abrasive
CN103571336A (en) * 2012-07-30 2014-02-12 张艺兵 Recycling and utilizing method of waste polishing powder
CN104371555A (en) * 2014-10-29 2015-02-25 安阳方圆研磨材料有限责任公司 Method for recycling waste rare earth polishing powder and rare earth polishing liquid
CN115418168A (en) * 2022-08-25 2022-12-02 萍乡泽昊新材料有限责任公司 Method for separating and extracting rare earth from waste rare earth polishing powder

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280175B (en) * 2006-04-07 2012-07-25 清美化学株式会社 Method for regenerating cerium-based abrasive
CN101899264A (en) * 2009-05-25 2010-12-01 甘肃稀土新材料股份有限公司 Rare earth polishing powder and preparation method thereof
CN101899281A (en) * 2009-05-25 2010-12-01 甘肃稀土新材料股份有限公司 Rare earth polishing powder and production method thereof
CN103079764A (en) * 2010-08-03 2013-05-01 Ranco株式会社 Method for regenerating ceria-based abrasive
CN102251117A (en) * 2011-06-17 2011-11-23 金华冠华水晶有限公司 Method for extracting rare earth component from crystal waste slag
CN102391833A (en) * 2011-09-08 2012-03-28 金华冠华水晶有限公司 Method for recycling and applying discarded rare earth polishing powder into crystal glass
CN103571336A (en) * 2012-07-30 2014-02-12 张艺兵 Recycling and utilizing method of waste polishing powder
CN103571336B (en) * 2012-07-30 2015-04-29 张艺兵 Recycling and utilizing method of waste polishing powder
CN102886308A (en) * 2012-10-15 2013-01-23 内蒙古科技大学 Method for recycling waste rare-earth polishing powder
CN102886308B (en) * 2012-10-15 2013-09-25 内蒙古科技大学 Method for recycling waste rare-earth polishing powder
CN104371555A (en) * 2014-10-29 2015-02-25 安阳方圆研磨材料有限责任公司 Method for recycling waste rare earth polishing powder and rare earth polishing liquid
CN104371555B (en) * 2014-10-29 2017-11-10 安阳方圆研磨材料有限责任公司 The method and rare earth polishing of useless polishing powder from rare earth reclaiming
CN115418168A (en) * 2022-08-25 2022-12-02 萍乡泽昊新材料有限责任公司 Method for separating and extracting rare earth from waste rare earth polishing powder

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