CN102337083A - Precision rare-earth polishing powder and preparation method thereof - Google Patents
Precision rare-earth polishing powder and preparation method thereof Download PDFInfo
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- CN102337083A CN102337083A CN2011102021507A CN201110202150A CN102337083A CN 102337083 A CN102337083 A CN 102337083A CN 2011102021507 A CN2011102021507 A CN 2011102021507A CN 201110202150 A CN201110202150 A CN 201110202150A CN 102337083 A CN102337083 A CN 102337083A
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Abstract
The invention provides precision rare-earth polishing powder and a preparation method thereof. The precision rare-earth polishing powder consists of the following components in percentage by mass: 5-50 percent of aluminosilicate and the balance of rare-earth oxide. Compared with the prior art, the precision rare-earth polishing powder and the preparation method of the precision rare-earth polishing powder provided by the invention have the advantages of low cost, simple production process, high product polishing ability, high wear resistance and the like.
Description
Technical field
The present invention relates to a kind of accurate polishing powder from rare earth and preparation method thereof, or rather, is about composite polishing powder from rare earth of a kind of silico-aluminate and rare earth oxide and preparation method thereof
Background technology
Polishing powder from rare earth is used for the polishing of lens, sheet glass, glass bulb, glasses, watchcase etc., has the advantages that polishing velocity is fast, precision is high.Since 20th century, invented polishing powder from rare earth the forties, turnout and application quantity increased gradually.The production technique of polishing powder from rare earth changes along with the progress of Rare Earth Separation technology.Along with the fast development of information industry, liquid-crystal display, plane demonstration, optical element etc. were more and more to the demand of polishing powder in recent years, and the polishing accuracy requirement is increasingly high.
It is raw material that early stage polishing powder from rare earth adopts hamartite, and like the CN1156749 of the clear U.S. of Japan chemical company, the CN1205354 patent is said, and developing into again afterwards with the mixed rare earth carbonate is that raw material is produced.Along with the reduction of Rare Earth Separation cost, adopt the higher rare earths material of cerium content to produce the cost that polishing powder from rare earth no longer increases polishing powder from rare earth, even its production cost is lower.
At present, widely used polishing powder from rare earth is that cerium oxide is the mishmetal oxyfluoride of staple on the market, has announced mixed rare-earth oxide, mixed rare earth fluoride, has used the abrasive material based on cerium of this material like CN101010402A; CN101284983A has announced a kind of ultra-fine, and spheroidizing rare-earth polish, this polishing powder from rare earth also are rare earth oxyfluoride.
The drawback that the polishing powder from rare earth that uses at present mainly exists is following: one, the proportion of polishing powder is bigger, and suspension is poor in the polishing powder use, has influenced the throwing erosion amount and the work-ing life of polishing powder from rare earth; Two, rare earth is a kind of Nonrenewable resources, uses pure rare earth to prepare polishing powder, is unfavorable for the Sustainable development of economy and society.
Summary of the invention
The object of the present invention is to provide a kind of accurate polishing powder from rare earth and preparation method thereof,, overcome the above-mentioned defective that prior art exists to satisfy the requirement of commerce to the polishing precision of production cost and increasingly stringent.
Described accurate polishing powder from rare earth is made up of silico-aluminate and rare earth oxide;
The mass percentage content of silico-aluminate is 5～50%, and all the other are rare earth oxide;
Preferably, the mass percentage content of silico-aluminate is 5～20%, and all the other are rare earth oxide;
Described silico-aluminate is one or more in kaolin, wilkinite, polynite, halloysite or the neusilin;
Described rare earth oxide is cerium oxide, cerium lanthanum oxide or cerium lanthanum oxide praseodymium;
The preparation method of described accurate polishing powder from rare earth may further comprise the steps:
(1) carbonated rare earth is used the acid dissolving, collect earth solution, silico-aluminate is joined in the earth solution, stir 0.5～1h, be heated to 40～80 ℃, get feed liquid A;
The mass percent of raw material is: silico-aluminate 2～33%, and it is a carbonated rare earth;
Preferably, silico-aluminate 2～10%, it is a carbonated rare earth;
Said carbonated rare earth is one or more in cerous carbonate, Phosbloc cerium or the carbonic acid La-Ce-Pr, and wherein, the TREO of cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr is 45%～48%, the CeO of cerous carbonate
2/ TREO＞99%, the CeO of Phosbloc cerium or carbonic acid La-Ce-Pr
2/ TREO is 60%～65%;
Described acid is a kind of in hydrochloric acid or the nitric acid;
Described silico-aluminate is selected from one or more in kaolin, wilkinite, polynite, halloysite or the neusilin;
(2) ammonium bicarbonate aqueous solution with 100～200g/L joins among the above-mentioned feed liquid A, and 1～2h is continued to stir in terminal point pH=7～8, and deposition gets slurries B;
(3) with above-mentioned slurries B dehydration, drying gets presoma C;
Described dewatering type is filter press, centrifugal or vacuum filtration;
(4) with above-mentioned presoma C at 950～1050 ℃ of roasting 3～6h, product of roasting;
(5) pulverize: with product of roasting through comminution by gas stream to D50:1.0～3 μ m, the accurate polishing powder from rare earth of title product.
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 pairing 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
Compared with prior art, accurate polishing powder from rare earth provided by the invention and preparation method thereof has that cost is low, production technique is simple, product is thrown erosion amount and wear resistance advantages of higher.
Description of drawings
Fig. 1 is the particle size distribution figure of the polishing powder of embodiment 1 preparation.
Fig. 2 is the particle size distribution figure of the polishing powder of Comparative Examples 4 preparations.
Embodiment
The granularity testing method is to adopt the laser particle analyzer of laser light scattering principle to record, and adopts Zhuhai American-European gram LS-POP (VI) type laser particle analyzer.
Under agitation condition, (REO is 45%, CeO with the 178g cerous carbonate
2/ TREO:99.1%) with nitric acid dissolve to pH=2, filter, clear solution;
With 10g kaolin, the 10g halloysite joins in the above-mentioned solution, stirs 0.5h post-heating to 40 ℃, slurries A;
Ammonium bicarbonate aqueous solution with 100g/L is added among the slurries A, and the pH of control terminal point is 7, gets slurries B;
With slurries B centrifuge dehydration, drying gets precursor C; With C behind 950 ℃ of roasting 5h, with product of roasting through comminution by gas stream to D50=2.99 μ m, the accurate polishing powder from rare earth of title product.
Wherein: the mass percentage content of silico-aluminate is 20%, and all the other are cerium oxide.
Under agitation condition, (TREO is 48%, CeO with 198g Phosbloc cerium
2/ TERO is 65%) with dissolving with hydrochloric acid to pH=2, filter, clear solution; With the 2.5g wilkinite, the 2.5g polynite joins in the above-mentioned solution, stirs 1h post-heating to 80 ℃, slurries A;
Ammonium bicarbonate aqueous solution with 200g/L is added among the slurries A, and the pH of control terminal point is 8, gets slurries B;
With slurries B centrifuge dehydration, drying gets precursor C; With C behind 1050 ℃ of roasting 3h, with product of roasting through comminution by gas stream to D50=1.8 μ m, the accurate polishing powder from rare earth of title product.
Wherein: the mass percentage content of silico-aluminate is 5%, and all the other are cerium lanthanum oxide.
Embodiment 3
Under agitation condition, (REO is 45%, CeO with the 111g cerous carbonate
2/ TREO be 99.5% usefulness nitric acid dissolve to pH=2, filter, clear solution; With the 5g neusilin, 15g kaolin, 30g wilkinite join to be chatted in the solution, stirs 0.5h post-heating to 40 ℃, slurries A; Ammonium bicarbonate aqueous solution with 100g/L is added among the slurries A, and the pH of control terminal point is 7, gets slurries B; With slurries B centrifuge dehydration, drying gets precursor C; With C behind 950 ℃ of roasting 6h, with product of roasting through comminution by gas stream to D50=1.2 μ m, the accurate polishing powder from rare earth of title product.
Wherein: the mass percentage content of silico-aluminate is 50%, and all the other are cerium oxide.
Embodiment 4
Under agitation condition, (REO is 47%, CeO with 192g carbonic acid La-Ce-Pr
2/ TERO is 60%) with nitric acid dissolve to pH=2, filter, clear solution; The 10g wilkinite is joined in the above-mentioned solution, stirs 0.5h post-heating to 40 ℃, slurries A; Ammonium bicarbonate aqueous solution with 100g/L is added among the slurries A, and the pH of control terminal point is 7, gets slurries B; With slurries B centrifuge dehydration, drying gets precursor C; With C behind 950 ℃ of roasting 5h, with product of roasting through comminution by gas stream to D50=2.99 μ m, the accurate polishing powder from rare earth of title product.
Wherein: the mass percentage content of silico-aluminate is 10%, and all the other are the cerium lanthanum oxide praseodymium.
Embodiment 5
Get polishing powder from rare earth 500g, add deionized water to 5L, getting concentration is the polishing fluid slurries of 100g/L.Adopt UNIPOL802 (Shenyang section is brilliant) precise grinding polisher that K9 glass is polished, automatic stirring to pulp, filtration cycle is used, and polishing arbor rotating speed is 120r/min, and pressure is 660N/cm
2, the polishing skin is KSP66B-1.25, polishing time is 6.5 hours, at regular intervals granularity of (first point is 0.5h, later on per hour once) test slurries and the dried weight of glass of record washing.Mass Calculation according to the polished front and back of take by weighing polishing element goes out difference, and this difference is divided by polishing time and throws the erosion amount, is designated as S respectively
h(h represents polishing time), MV are S
a, concrete numerical value is seen table 1.
Table 1
| S 0.5 | S 1.5 | S 2.5 | S 3.5 | S 4.5 | S 5.5 | S 6.5 | Sa | |
| Embodiment 1 | 2.46 | 2.36 | 2.63 | 2.38 | 2.76 | 2.59 | 2.59 | 2.54 |
| |
1.80 | 2.01 | 2.19 | 2.16 | 2.12 | 2.15 | 2.18 | 2.09 |
| Embodiment 3 | 1.93 | 2.31 | 2.51 | 2.48 | 2.48 | 2.53 | 2.49 | 2.39 |
| Embodiment 4 | 1.98 | 2.01 | 2.09 | 2.06 | 2.12 | 2.05 | 2.11 | 2.06 |
Claims (5)
1. accurate polishing powder from rare earth is characterized in that, is made up of silico-aluminate and rare earth oxide;
The mass percentage content of silico-aluminate is 5～50%, and all the other are rare earth oxide.
2. accurate polishing powder from rare earth according to claim 1 is characterized in that, the mass percentage content of silico-aluminate is 5～50%, and all the other are rare earth oxide.
3. accurate polishing powder from rare earth according to claim 1 and 2 is characterized in that, described silico-aluminate is one or more in kaolin, wilkinite, polynite, halloysite or the neusilin; Described rare earth oxide is cerium oxide, cerium lanthanum oxide or cerium lanthanum oxide praseodymium.
4. the preparation method of accurate polishing powder from rare earth according to claim 1 and 2 may further comprise the steps:
(1) carbonated rare earth is dissolved with acid, collect earth solution, silico-aluminate is joined in the earth solution, be heated with stirring to 40～80 ℃, get feed liquid A;
The mass percent of raw material is: silico-aluminate 2～33%, and it is a carbonated rare earth;
Said carbonated rare earth is one or more in cerous carbonate, Phosbloc cerium or the carbonic acid La-Ce-Pr, and wherein, the TREO of cerous carbonate, Phosbloc cerium or carbonic acid La-Ce-Pr is 45%～48%, the CeO of cerous carbonate
2/ TREO＞99%, the CeO of Phosbloc cerium or carbonic acid La-Ce-Pr
2/ TREO is 60%～65%;
Described acid is a kind of in hydrochloric acid or the nitric acid;
Described silico-aluminate is selected from one or more in kaolin, wilkinite, polynite, halloysite or the neusilin;
(2) ammonium bicarbonate aqueous solution with 100～200g/L joins among the above-mentioned feed liquid A, and terminal point pH=7～8 continue to stir, and deposition gets slurries B;
(3) with above-mentioned slurries B dehydration, drying gets presoma C;
(4) with above-mentioned presoma C at 950～1050 ℃ of roasting 3～6h, product of roasting;
(5) pulverize: with product of roasting through comminution by gas stream to D50:1.0～3 μ m, the accurate polishing powder from rare earth of title product.
5. method according to claim 4 is characterized in that, the mass percent of raw material is: silico-aluminate 2～33%, it is a carbonated rare earth.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103254870A (en) * | 2013-05-19 | 2013-08-21 | 郭尧 | Lanthanum-cerium oxide rear-earth polishing powder and preparation method thereof |
| CN103555206A (en) * | 2013-10-22 | 2014-02-05 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| WO2014071859A1 (en) * | 2012-11-07 | 2014-05-15 | 有研稀土新材料股份有限公司 | Cerium oxide based composite polishing powder and preparation method thereof |
| CN104562019A (en) * | 2015-01-09 | 2015-04-29 | 西南石油大学 | Environment-friendly acidic chemical polishing solution and chemical polishing method |
| CN106281044A (en) * | 2016-08-09 | 2017-01-04 | 西安博尔新材料有限责任公司 | A kind of preparation method of floating type aqueous polishing liquid |
| CN106675416A (en) * | 2016-11-30 | 2017-05-17 | 安徽电气集团股份有限公司 | Rare earth material polishing powder |
| CN108659714A (en) * | 2018-05-11 | 2018-10-16 | 内蒙古包钢和发稀土有限公司 | The production method of Rare earth oxide polishing powder raw material |
| CN115304407A (en) * | 2022-09-29 | 2022-11-08 | 天津包钢稀土研究院有限责任公司 | Application of ineffective rare earth polishing powder in preparation of radiation material |
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| US20070042894A1 (en) * | 2005-08-17 | 2007-02-22 | Aitken Bruce G | High strain point glasses |
| CN1837043A (en) * | 2006-04-14 | 2006-09-27 | 西北师范大学 | Rare earth particle and montmorillonite nano composite materials and process for preparing same |
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| US9725620B2 (en) | 2012-11-07 | 2017-08-08 | Grirem Advanced Materials Co., Ltd. | Cerium oxide based composite polishing powder and preparation method thereof |
| WO2014071859A1 (en) * | 2012-11-07 | 2014-05-15 | 有研稀土新材料股份有限公司 | Cerium oxide based composite polishing powder and preparation method thereof |
| CN104884556A (en) * | 2012-11-07 | 2015-09-02 | 有研稀土新材料股份有限公司 | Cerium oxide based composite polishing powder and preparation method thereof |
| CN104884556B (en) * | 2012-11-07 | 2017-09-26 | 有研稀土新材料股份有限公司 | A kind of cerium oxide base compound polishing powder and preparation method thereof |
| CN103254870A (en) * | 2013-05-19 | 2013-08-21 | 郭尧 | Lanthanum-cerium oxide rear-earth polishing powder and preparation method thereof |
| CN103555206A (en) * | 2013-10-22 | 2014-02-05 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN103555206B (en) * | 2013-10-22 | 2015-07-08 | 上海华明高纳稀土新材料有限公司 | Rare earth polishing powder and preparation method thereof |
| CN104562019A (en) * | 2015-01-09 | 2015-04-29 | 西南石油大学 | Environment-friendly acidic chemical polishing solution and chemical polishing method |
| CN104562019B (en) * | 2015-01-09 | 2017-04-12 | 西南石油大学 | Environment-friendly acidic chemical polishing solution and chemical polishing method |
| CN106281044A (en) * | 2016-08-09 | 2017-01-04 | 西安博尔新材料有限责任公司 | A kind of preparation method of floating type aqueous polishing liquid |
| CN106675416A (en) * | 2016-11-30 | 2017-05-17 | 安徽电气集团股份有限公司 | Rare earth material polishing powder |
| CN108659714A (en) * | 2018-05-11 | 2018-10-16 | 内蒙古包钢和发稀土有限公司 | The production method of Rare earth oxide polishing powder raw material |
| CN108659714B (en) * | 2018-05-11 | 2020-11-13 | 内蒙古包钢和发稀土有限公司 | Production method of rare earth oxide polishing powder raw material |
| CN115304407A (en) * | 2022-09-29 | 2022-11-08 | 天津包钢稀土研究院有限责任公司 | Application of ineffective rare earth polishing powder in preparation of radiation material |
| CN115304407B (en) * | 2022-09-29 | 2022-12-27 | 天津包钢稀土研究院有限责任公司 | Application of ineffective rare earth polishing powder in preparation of radiation material |
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Effective date of registration: 20181211 Address after: 3802 Shengang Road, Songjiang District, Shanghai, 20161 Patentee after: Fang Fu (Shanghai) new Mstar Technology Ltd Address before: 201613 No. 81, Fan Hua Road, Songjiang District, Shanghai Patentee before: Shanghai Huaming Gona Rare Earth New Materials Co., Ltd. |
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