CN103215012B - Preparation method for regenerating rear-earth polishing powder - Google Patents
Preparation method for regenerating rear-earth polishing powder Download PDFInfo
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- CN103215012B CN103215012B CN201310148306.7A CN201310148306A CN103215012B CN 103215012 B CN103215012 B CN 103215012B CN 201310148306 A CN201310148306 A CN 201310148306A CN 103215012 B CN103215012 B CN 103215012B
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- rare earth
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Abstract
The invention discloses a preparation method for regenerating rear-earth polishing powder. The preparation method comprises the following processes: (1) mixing the waste rear-earth polishing powder and adopting a shaker reselecting device for reselecting and separating to obtain heavy constituents; (2) treating the reselected rear-earth polishing powder by 2%-25% (in percentage by weight) of ammonium fluozirconate aqueous solution; heating up to 50 DEG C to 75 DEG C; stirring and reacting for 6-12 hours; and settling, cleaning and filtering to recycle solid; and (3) preparing regenerated rear-earth polishing powder, wherein the primarily generated rear-earth polishing powder is primarily dried, roasted for 3-10 hours at 1000 DEG C to 1100 DEG C, cooled, crushed by gas flow to obtain the regenerated rear-earth polishing powder which can reach a grain size range for being reused as the polishing powder. The preparation method for regenerating rear-earth polishing powder has the advantages of being less in using amount of chemical substances, simple in process, easy to control conditions, low in production cost, easy to realize industrial production, high in recovery rate, good in powder polishing effect and the like.
Description
Technical field
What the present invention relates to is a kind for the treatment of process that waste and old resource is recycled, particularly the preparation method of a kind of system to fail rare earth polishing powder regeneration.
Background technology
Polishing powder from rare earth, for the polishing of lens, sheet glass, televisor glass bulb, ophthalmic lens, ambetti goods, watchcase, precision optical instrument element etc., has the advantages that polishing velocity is fast, precision is high.Process by means such as cut mechanically, grinding, polishings, in the course of processing, polishing is a very important link, can improve surface property and the optical property of various goods by polishing, polishing is at present mainly to rely on polishing powder from rare earth to complete.The polishing powder from rare earth production in the whole world is about 20,000 tons, and on the whole the turnout of the polishing powder from rare earth of China and application quantity equate, produce every year 10000 tons of left and right, wherein domestic personal 8000 tons, exports 2000 tons.Produce thus a large amount of useless polishing powder from rare earth.Have a lot of factories using discarded polishing powder from rare earth as waste product, be deposited near plant area, this is contaminate environment, land occupation not only, and is the waste to rare earth resources.
Now widely used 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 closely related.The major cause that polishing powder from rare earth lost efficacy is: the firstth, and in polishing process, have a large amount of glass granules and be enriched on rare earth oxide surface, also have sneaking into of greasy dirt and macrobead foreign matter, reduce the content of rare earth oxide, make polishing powder in polishing process, reduce heat of friction, reduce the plastic degeneration of glass surface, affected glass surface molecule and redistribute and form the process of flat surface.The secondth, polishing process is a kind of strong process of lapping, causes polishing crystal grain by undue refinement, has reduced polishing effect.
In order to address the above problem, be necessary to study the regeneration techniques of polishing powder from rare earth, both can reduce environmental pollution, make full use of rare earth resources, can reduce production costs again.About polishing powder from rare earth regeneration, related documents also has report.A kind of renovation process of fail rare earth polishing powder is disclosed in Chinese patent CN1246407C, the method is for the polishing powder from rare earth losing efficacy, regeneration techniques has been proposed, the method has proposed direct the rare earth polishing of losing efficacy powder to adopt the water-soluble alkali of 0.5 ~ 3mol/L and the chemical reagent of soluble fluoride to carry out chemical treatment, so consume a large amount of chemical reagent, uneconomical, and produce a large amount of waste water, can bring environmental pollution, do not relate to going out of other component yet, then reclaim solid thermal processing, applicable scope is restricted.In Chinese patent CN1194060C, disclose a kind of renovation process of the polishing powder from rare earth of regenerating, the method is that useless polishing powder from rare earth is added in acid, by trivalent rare earth oxide dissolution, CeO
2do not dissolve and add again 30% hydrogen peroxide by CeO
2dissolve, then add 5 ~ 8% light rare earths oxyhydroxide or Ce(OH)
4suspension, be that rare earth redeposition divides, this dissolving rare earth and oxide-reduction method, realize polishing powder from rare earth regeneration, therefore consume a large amount of chemical reagent, uneconomical, and produce a large amount of waste water, can bring environmental pollution, and the solubleness of rare earth oxide is very low, the rate of recovery is very low.Chinese Patent Application No. is a kind of method that discloses regeneration in 201110265136.1 and be applied to the discarded polishing powder from rare earth of crystal glass, and the method adopts (1) to utilize screening plant to carry out scalping to polishing powder from rare earth waste residue and removes foreign material and macrobead; (2) polishing powder from rare earth waste residue is sized mixing, utilize gravitational separation equipment to carry out gravity treatment, separate the polishing powder from rare earth waste that the restructuring obtaining is divided into high-content; (3) carrying out chemical treatment dissolving solvend wherein with strong acid; (4) waste through 800 DEG C of above high-temperature roastings.The method strong acid used is nitric acid and hydrofluoric acid, while use, can dangerously will take care due to the special property of hydrofluoric acid.
At present, in the report about discarded polishing powder from rare earth renovation process, there is the method that the salt that utilizes fluorochemicals dissolves to remove glass ingredient, also have to utilize and dissolve rare earth and redox method, realize polishing powder from rare earth regeneration.After utilizing in addition physical method for separation, going deimpurity method with strong acid.These methods all, by consuming the chemical substances such as a large amount of strong acid and strong bases, are brought significant cost, uneconomical, but also can produce a large amount of waste water, pollute.Therefore, in order effectively to make polishing powder from rare earth regeneration, do not produce new pollution, be necessary to study new renovation process, can highly efficient regeneration polishing powder from rare earth, free from environmental pollution again, the object that the present invention that Here it is will reach.
Summary of the invention
The object of this invention is to provide a kind of preparation method of polishing powder from rare earth regeneration, efficiently make discarded polishing powder from rare earth recover polishing performance, and do not produce pollution.
Object of the present invention is achieved through the following technical solutions.
A preparation method for polishing powder from rare earth regeneration, is characterised in that the method has following processing step:
(1) gravity treatment polishing powder from rare earth: discarded polishing powder from rare earth is sized mixing, and the concentration of sizing mixing is 25 ~ 35% mass percents, adopts table concentration equipment to carry out Gravity separation, separates the heavy constituent obtaining, and attaches most importance to and selects polishing powder from rare earth through super-dry;
(2) preparation of nascent polishing powder from rare earth: gravity treatment polishing powder from rare earth is closed to zirconic acid aqueous ammonium with the hexafluoro that mass percent is 2 ~ 25% and process, heat 50 ~ 75 DEG C, stirring reaction 6 ~ 12 h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, at 1000 DEG C ~ 1100 DEG C roasting 3 ~ 12 h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50;
The inventive method core is: 1) utilize gravitational separation equipment to discarded polishing powder from rare earth gravity treatment, most of impurity is all separated, this is physical method environmentally safe, has also reduced chemical treatment difficulty; 2) adopt hexafluoro to close zirconic acid ammonium and process gravity treatment polishing powder from rare earth, have following decomposition reaction the heat a little in the situation that because hexafluoro closes zirconic acid ammonium: (NH
4)
2[ZrF
6]=ZrF
4+ NH
3+ 2HF, the hydrofluoric acid of decomposition forms equal phase concentration in system, can fully and uniformly the impurity in gravity treatment polishing powder from rare earth be disposed to residual ZrF
4and NH
3in 1000 DEG C of roastings, volatilize, ZrF
4some is converted into ZrO
2particle, has due to ZrO
2also be very good polishing material, its existence has strengthened the polishing performance of regeneration polishing powder; 3) be to remove thermosetting resin and the organic greasy dirt do not disposed 1000 DEG C ~ 1100 DEG C roastings, and improve the hardness of polishing powder.
Particle size test method of the present invention is the granularity equivalent diameter size that adopts laser particle analyzer to record.
Advantage of the present invention and effect are:
(1) chemical substance consumption of the present invention is few, has reduced the pollution to environment, and chemical substance hexafluoro used closes zirconic acid ammonium can dispose the impurity in discarded polishing powder, can in polishing powder, increase again ZrO
2, the polishing performance of polishing powder is improved, it is little that the polishing powder of regeneration has meso-position radius grain, the feature that particle size distribution is narrow.
(2) technique of the present invention is simple, and condition is easy to control, and production cost is low, is easy to suitability for industrialized production.
(3) rate of recovery of polishing powder from rare earth of the present invention is high, and powder polishing effect is good, and polishing performance can return in 97.2 ~ 99.67% original scopes.
(4) the applicable various polishing powder from rare earth regeneration of the present invention.
Embodiment
Embodiment 1
(1) gravity treatment polishing powder from rare earth: get the discarded polishing powder from rare earth of 30kg, remove macrobead thing and foreign matter by 60 order sieve.After sieving, thin component is sized mixing, and the mass percent concentration of sizing mixing is 25% slurries, adopts 1m
2on shaking table, carry out Gravity separation, collect heavy constituent.Through super-dry, obtain gravity treatment polishing powder from rare earth, by Weighing and analytical test, result shows, and rare earth yield is 72.6%, and Purity of Rare Earth is 79.2%;
(2) preparation of nascent polishing powder from rare earth: get the gravity treatment polishing powder from rare earth of 500g oven dry in 1000mL beaker, adding 500mL mass percent is that 10% hexafluoro closes zirconic acid aqueous ammonium, stir, intensification is heated to 50 DEG C, stirring reaction 8 h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, and put into High Temperature Furnaces Heating Apparatus, temperature rises at 1000 DEG C of roasting 4 h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50, by Weighing and analytical test, result shows, and rare earth yield is 98%, and Purity of Rare Earth is 90%.
Embodiment 2
(1) gravity treatment polishing powder from rare earth: get the discarded polishing powder from rare earth of 30kg, remove macrobead thing and foreign matter by 60 order sieve.After sieving, thin component is sized mixing, and the mass percent concentration of sizing mixing is 35% slurries, adopts 1m
2on shaking table, carry out Gravity separation, collect heavy constituent.Through super-dry, obtain gravity treatment polishing powder from rare earth, by Weighing and analytical test, result shows, and rare earth yield is 73.6%, and Purity of Rare Earth is 80.2%;
(2) preparation of nascent polishing powder from rare earth: get the gravity treatment polishing powder from rare earth of 300g oven dry in 1000mL beaker, adding 500mL mass percent is that 8% hexafluoro closes zirconic acid aqueous ammonium, stir, intensification is heated to 60 DEG C, stirring reaction 10 h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, and put into High Temperature Furnaces Heating Apparatus, temperature rises at 1100 DEG C of roasting 6 h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50, by Weighing and analytical test, result shows, and rare earth yield is 98.2%, and Purity of Rare Earth is 89%.
Embodiment 3
(1) gravity treatment polishing powder from rare earth: get the discarded polishing powder from rare earth of 30kg, remove macrobead thing and foreign matter by 60 order sieve.After sieving, thin component is sized mixing, and the mass percent concentration of sizing mixing is 30% slurries, adopts 1m
2on shaking table, carry out Gravity separation, collect heavy constituent.Through super-dry, obtain gravity treatment polishing powder from rare earth, by Weighing and analytical test, result shows, and rare earth yield is 71.8%, and Purity of Rare Earth is 81.2%;
(2) preparation of nascent polishing powder from rare earth: get the gravity treatment polishing powder from rare earth of 500g oven dry in 1000mL beaker, adding 600mL mass percent is that 5% hexafluoro closes zirconic acid aqueous ammonium, stir, intensification is heated to 70 DEG C, stirring reaction 12 h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, and put into High Temperature Furnaces Heating Apparatus, temperature rises at 1000 DEG C of roasting 12 h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50, by Weighing and analytical test, result shows, and rare earth yield is 96.8%, and Purity of Rare Earth is 91%;
Embodiment 4
(1) gravity treatment polishing powder from rare earth: get the discarded polishing powder from rare earth of 30kg, remove macrobead thing and foreign matter by 60 order sieve.After sieving, thin component is sized mixing, and the mass percent concentration of sizing mixing is 30% slurries, adopts 1m
2on shaking table, carry out Gravity separation, collect heavy constituent.Through super-dry, obtain gravity treatment polishing powder from rare earth, by Weighing and analytical test, result shows, and rare earth yield is 71.8%, and Purity of Rare Earth is 81.2%;
(2) preparation of nascent polishing powder from rare earth: get the gravity treatment polishing powder from rare earth of 400g oven dry in 1000mL beaker, adding 400mL mass percent is that 20% hexafluoro closes zirconic acid aqueous ammonium, stir, intensification is heated to 50 DEG C, stirring reaction 6h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, and put into High Temperature Furnaces Heating Apparatus, temperature rises at 1000 DEG C of roasting 8h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50, by Weighing and analytical test, result shows, and rare earth yield is 96.8%, and Purity of Rare Earth is 91%.
Embodiment 5
(1) gravity treatment polishing powder from rare earth: get the discarded polishing powder from rare earth of 30kg, remove macrobead thing and foreign matter by 60 order sieve.After sieving, thin component is sized mixing, and the mass percent concentration of sizing mixing is 25% slurries, adopts 1m
2on shaking table, carry out Gravity separation, collect heavy constituent.Through super-dry, obtain gravity treatment polishing powder from rare earth, by Weighing and analytical test, result shows, and rare earth yield is 72.6%, and Purity of Rare Earth is 79.2%;
(2) preparation of nascent polishing powder from rare earth: get the gravity treatment polishing powder from rare earth of 500g oven dry in 1000mL beaker, adding 500mL mass percent is that 12% hexafluoro closes zirconic acid aqueous ammonium, stir, intensification is heated to 60 DEG C, stirring reaction 8 h, then by reclaiming solid after sedimentation, cleaning and filtration, obtain nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, and put into High Temperature Furnaces Heating Apparatus, temperature rises at 1050 DEG C of roasting 10h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0 ~ 5.0 μ m, D
10>=0.5 D
50, D
95≤ 2D
50, D
100≤ 3D
50, by Weighing and analytical test, result shows, and rare earth yield is 97.2%, and Purity of Rare Earth is 90%.
Polishing performance test, the regenerate polishing ability 59.6(of polishing powder from rare earth product of embodiment 1 is worn away amount of glass mg/10min); The regenerate polishing ability 59.1 of polishing powder from rare earth product of embodiment 2; The regenerate polishing ability 60.1 of polishing powder from rare earth product of embodiment 3; The regenerate polishing ability 59.8 of polishing powder from rare earth product of embodiment 4; The regenerate polishing ability 60.6 of polishing powder from rare earth product of embodiment 5; The polishing ability 60.8 of former polishing powder from rare earth product; As can be seen here, the regenerate polishing ability of polishing powder from rare earth of the present invention returns to former polishing powder polishing ability in 97.2 ~ 99.67% scopes, illustrates that the method effect is fine.
Claims (2)
1. a preparation method for polishing powder from rare earth regeneration, is characterized in that the method has following processing step:
(1) gravity treatment polishing powder from rare earth: discarded polishing powder from rare earth is sized mixing, and the concentration of sizing mixing is 25～35% mass percents, adopts table concentration equipment to carry out Gravity separation, separates the heavy constituent obtaining, and attaches most importance to and selects polishing powder from rare earth through super-dry;
(2) preparation of nascent polishing powder from rare earth: gravity treatment polishing powder from rare earth is closed to zirconic acid aqueous ammonium with the hexafluoro that mass percent is 2～25% and process, heat 50～75 DEG C, stirring reaction 6～12h, then by reclaiming solid after sedimentation, cleaning and filtration, obtains nascent polishing powder from rare earth;
(3) regeneration polishing powder from rare earth preparation: will come into being polishing powder from rare earth after preliminarily dried, at 1000 DEG C～1100 DEG C roasting 3～12h, cooling after, through comminution by gas stream, obtain regeneration polishing powder from rare earth, the D of the regeneration polishing powder from rare earth obtaining
50particle diameter is 1.0～5.0 μ m, D
10>=0.5D
50, D
95≤ 2D
50, D
100≤ 3D
50.
2. according to the preparation method of a kind of polishing powder from rare earth regeneration described in claim 1, it is characterized in that: it is more than chemical pure that the hexafluoro described in step (2) closes zirconic acid ammonium.
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|---|---|---|---|
| CN201310148306.7A CN103215012B (en) | 2013-04-26 | 2013-04-26 | Preparation method for regenerating rear-earth polishing powder |
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|---|---|---|---|
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| CN103215012B true CN103215012B (en) | 2014-07-02 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962200A (en) * | 2015-07-23 | 2015-10-07 | 西安西光精细化工有限公司 | Recovery preparation method of waste rare-earth polishing powder |
| CN107099254A (en) * | 2017-05-02 | 2017-08-29 | 王丹 | A kind of method of ornaments crystal glass polishing powder from rare earth regeneration |
| CN110241309B (en) * | 2019-05-08 | 2020-06-19 | 湖南景翌湘台环保高新技术开发有限公司 | Method for extracting white carbon black and rare earth water purifying agent from waste rare earth polishing powder |
| CN114276754A (en) * | 2022-01-25 | 2022-04-05 | 单立 | Polishing powder is with retrieving regeneration facility |
| CN115820130B (en) * | 2023-01-05 | 2024-05-28 | 包头稀土研究院 | Regeneration method of rare earth polishing powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456624A (en) * | 2003-03-10 | 2003-11-19 | 田汝梅 | Fail rare earth polishing powder reproducing method |
| CN102925060A (en) * | 2012-11-09 | 2013-02-13 | 济南大学 | Preparation method of marble composite polishing powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1456624A (en) * | 2003-03-10 | 2003-11-19 | 田汝梅 | Fail rare earth polishing powder reproducing method |
| CN102925060A (en) * | 2012-11-09 | 2013-02-13 | 济南大学 | Preparation method of marble composite polishing powder |
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