CN104060111B - A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue - Google Patents
A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue Download PDFInfo
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Abstract
The present invention discloses a kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue, the technical scheme utilizing sectional type to extract realizes component sorting for the inefficacy polishing powder particle in polishing powder waste residue, from inefficacy polishing powder particle, extract La, Pr element one section of link, from inefficacy polishing powder particle, extract Ce element two sections of links; Based on two stage process flow process, rare earth element sharpening Separation and Recovery can be realized simultaneously; And by the impurity component of chemical process in different process sections removes wherein waste residue respectively and impurity element, thus guarantee the high physical index of product.The invention provides a kind of method that resource efficiency is high, processing condition are gentle, technical process is easy, product meets high physical index.
Description
Technical field
The present invention relates to a kind of method of recovering rare earth element from polishing powder from rare earth waste residue, belong to the technical field of waste resource comprehensive utilization.
Background technology
Polishing powder from rare earth, because of the Wuli-Shili-Renli system approach of its uniqueness and excellent polishing performance, is widely used in the precise polished of display screen, electronic glass, opticglass, ornaments, building materials, mould and precision instrument.The polishing powder from rare earth of current main application is cerium base class polishing powder, because its polishing velocity is fast, smooth finish, planeness are high advantage is widely used in the polishing of glass substrate of optical lens, liquid-crystal display, panel computer, mobile phone faceplate, making hard disk.The Large-scale enterprises about 15 that current domestic existing cerium-based rare earth polishing powder is produced, yearly capacity about 1.6 ten thousand tons, actual consumption rare earth more than 1.4 ten thousand tons (REO).According to the analytic statistics to polishing powder from rare earth product main on domestic market, polishing powder from rare earth middle-weight rare earths total amount (TREO)>=86wt%, wherein: CeO
2/ TREO>=55%, La
2o
3/ TREO=19 ~ 36%, Pr
6o
11/ TREO=4 ~ 7%.
First polishing powder from rare earth wants furnishing slurries with water in use often, and solid content is generally between 5 ~ 20wt%; Along with the increase of polishing slurries recycle number of times, polishing powder particle can constantly be worn and torn until lost efficacy; Meanwhile, the base material (as glass, stone material etc.) of polishing is also along with polishing process in continuous enrichment in slurry system.Because production technique reason, above-mentioned cerium-based rare earth polishing powder finally all inevitably becomes a class trade waste in polishing use procedure, collects after press filtration with the form of " polishing powder from rare earth waste residue ".In general, polishing powder from rare earth waste residue comprises following 4 class components: the cerium-based rare earth polishing powder particle 1) lost efficacy; 2) the base material chip chipped away is thrown, as glass micro mist, stone material chip etc.; 3) thing under the throwing of polishing pad is derived from, as wool pad, foam bits etc.; 4) precipitation agent, as aluminum chloride etc.On the whole, along with the increase of domestic polishing powder from rare earth turnout and consumption, the required Rare-earth Mine mineral products resource consumed can get more and more on the one hand, on the other hand, in use formed polishing powder from rare earth waste residue also in continuous increase, and is the main solid waste source in polishing industry always.Meanwhile, in polishing powder from rare earth waste residue, be rich in a large amount of rare earth elements, there is valuable resource utilization recovery value.Therefore, the extraction carrying out rare earth element from polishing powder from rare earth waste residue is reclaimed, and has just become an important technology and industry problem.
Domestic patent " a kind of recovery and reuse method of polishing powder from rare earth waste residue and liquid " (patent No.: 201110053793.X), " a kind of recovery and reuse method of polishing powder from rare earth waste residue and liquid " (application number: the renovation process 201310233211.5) disclosing fail rare earth polishing powder, the method is by the physical chemistry process to fail rare earth polishing powder, polishing powder effective constituent regeneration polishing powder is wherein used, and rare earth element is not wherein extracted and be used.Applicant is at " a kind of devices and methods therefor realizing the online recycle of polishing powder from rare earth waste material " (application number: 201410190144.8), provide two kinds of technical schemes of useless polishing powder from rare earth rapid regeneration and online recycle in " a kind of realize the method that useless polishing powder from rare earth cleans rapid regeneration " (application number: 201410189852.X), but equally also do not relate to the technique content of recovering rare earth element from useless polishing powder from rare earth.The domestic patent method of useless rare earth abrasive substance recovering rare earth element " a kind of by " (application number: 201110224407.9) adopt the tertiary mixture of ammonium chloride, magnesium sulfate, sulfuric acid to leach as decomposition agent, technique realization condition is quite harsh, and process waste ratio is also quite large.Domestic patent " a kind of method producing lanthanum oxalate cerium from polishing powder from rare earth the waste residue " (patent No.: 201210155031.5) adopt the vitriol oil to carry out to waste residue leachings and process thus recovering rare earth element, have in actual application that process costs is higher, vitriol oil consumption is bigger than normal, product cannot guarantee the limitation such as purity requirement.Domestic patent " a kind of method producing rare earth oxide from polishing powder from rare earth waste residue " (application number: 201310063829.1) adopt alkali roasting, then carry out the technical scheme of hcl acidifying, finally obtain two class cerium lanthanum oxide mixtures, its technique realizes comparatively numerous and diverse, and process costs is high, process waste ratio is large.Therefore, more economy, Production Flow Chart are more easy to invent a kind of manufacturing process, have more the novel method that industrial technology is worth on the whole, to the industrialization technology level promoted from polishing powder from rare earth waste residue recovering rare earth element, the high added value recycle of serving polishing powder from rare earth waste residue middle-weight rare earths resource is of great practical significance.
Summary of the invention
The object of the invention is, for all deficiencies of existing polishing powder from rare earth rare earth elements recovery technology, to provide a kind of method that resource efficiency is high, processing condition are gentle, technical process is easy, product meets high physical index.Inventor herein conducts in-depth research, find that the technical scheme utilizing sectional type to extract can realize component sorting for the inefficacy polishing powder particle in polishing powder waste residue, from inefficacy polishing powder particle, extract La, Pr element one section of link, from inefficacy polishing powder particle, extract Ce element two sections of links; Based on two stage process flow process, rare earth element sharpening Separation and Recovery can be realized simultaneously; And remove impurity component in waste residue and impurity element by chemical process respectively at different process sections, thus guarantee the high physical index of product.The advantageous effects of comprehensive above-mentioned several respects, thus complete the present invention.
In order to the technical scheme of the present invention of statement clearly, first set forth each component thing characteristic in domestic polishing powder from rare earth waste residue.By the proximate analysis of domestic main polishing powder from rare earth, and the analysis to glossing and polishing process, can understand polishing powder from rare earth waste residue component complicated, all kinds of component thing and quality event thereof are described as follows:
1) the cerium-based rare earth polishing powder particle lost efficacy.Polishing powder from rare earth particle is topmost composition thing in waste residue.In polishing process, just particle attenuates, diminishes, and throws and cuts performance reduction and then lost efficacy, and the rare earth element composition of polishing powder from rare earth does not change, basically identical with original polishing powder component, that is: total amount of rare earth (TREO)>=86wt%, wherein CeO
2/ TREO>=55%, La
2o
3/ TREO=19 ~ 36%, Pr
6o
11/ TREO=4 ~ 7%;
2) the base material chip chipped away is thrown, as glass micro mist, stone material chip etc.; Main component is SiO
2and silicate glass, calcium carbonate, and calcium, magnesium oxide;
3) thing under the throwing of polishing pad is derived from, as wool pad, foam bits etc.; Main component is the impurity of organism class, can be removed easily by the method for physical separation;
4) precipitation agent, as aluminum chloride etc.
The object of the present invention is achieved like this: a kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue, is characterized in that the method comprises the following steps:
(1) polishing powder from rare earth waste residue is carried out physical separation, remove foreign material;
(2) one segment units: the hydrochloric acid adding 5 ~ 12mol/L in polishing powder waste residue carries out an acidolysis, control temperature is room temperature or 50 ~ 80 DEG C, obtains being rich in one section of leach liquor of La, Pr element and being rich in one section of filter residue of Ce element after being separated by filtration; The add-on of hydrochloric acid is determined by the content situation of La, Pr, Ca, Mg, Al element in waste residue, all form 1.1 ~ 2.5 times of muriatic theoretical demand molar weight by above-mentioned element and add hydrochloric acid, react and compare one section of filter residue rare earth element total amount with lanthanum praseodymium element residual in one section of filter residue and be less than 0.3% for terminal; In one section of leach liquor, add the salt of containing sulfate radicals, being separated and removing Ca, Mg element throw out, no longer there is CaSO in the add-on of the salt of containing sulfate radicals
4, MgSO
4white precipitate be terminal; Regulate the pH value of one section of leach liquor to 3 ~ 4.5 by alkali again, be separated and remove Al element throw out; For section removal of impurities liquid of after above-mentioned removal of impurities, one of following method is adopted to obtain rare earth compound corresponding to La and Pr element:
Method one: obtain lanthanum oxalate and praseodymium oxalate after extracting and separating, oxalic acid precipitation, drying;
Method two: obtain lanthanum oxalate praseodymium after oxalic acid precipitation, drying;
Method three: obtain lanthanum trioxide and Praseodymium trioxide after extracting and separating, precipitation, calcination;
Method four: obtain lanthanum praseodymium oxide after precipitation, calcination;
(3) two segment units: add the vitriol oil and carry out secondary acidolysis in the one section of filter residue being rich in Ce, control temperature of reaction at 150 ~ 300 DEG C, in 2 ~ 8 hours reaction times, obtain two sections of leach liquors and two sections of filter residues after being separated by filtration; The add-on of the vitriol oil is determined by Ce content in one section of filter residue, by CeO in one section of filter residue
21.1 ~ 1.6 times that are all converted into the theoretical demand molar weight of ceric sulfate add the vitriol oil; For above-mentioned two sections of leach liquors, one of following method is adopted to obtain rare earth compound corresponding to Ce element:
Method five: obtain Sedemesis after oxalic acid precipitation, drying;
Method six: obtain cerium oxide after precipitation, high-temperature calcination.
Below invention is described further:
The method of a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue of the present invention, is characterized in that: described polishing powder from rare earth waste residue refers to the polishing powder waste residue of the total amount of the rare earth oxide after for liquid crystal display, opticglass, stone material, Crystal ornaments polishing at more than 10wt%.
The method of a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue of the present invention, is characterized in that: the salt of step (2) described containing sulfate radicals is the one in sodium sulfate, potassium sulfate, ammonium sulfate; Described alkali is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
The method of a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue of the present invention, is characterized in that: the vitriol oil described in step (3) to be massfraction be 98% the vitriol oil.
Know-why of the present invention is:
1, by Ce(IV in polishing powder from rare earth waste residue), La(III), Pr(III) etc. the further investigation of rare earth element response characteristic, by hydrochloric acid, the vitriol oil carry out respectively an acidolysis, secondary acidolysis and reach rare earth element segmentation leach technical object, effectively can improve the decomposition leaching yield of polishing powder particle rare earth elements; From inefficacy polishing powder particle, extract La, Pr element one section of link, from inefficacy polishing powder particle, extract Ce element two sections of links, thus complete sharpening separation between La, Pr and Ce element.
2, on the basis that segmentation is leached, by disposing the removal of impurities of leach liquor, avoiding the quality influence of the elements such as Ca, Mg, Al to rare-earth products, guaranteeing the high physical index of rare-earth products.
Compared with prior art, its advantage is in the present invention:
1, the present invention does not need the acid that use HF acid, nitric acid etc. are larger to environmental hazard, but adopt hydrochloric acid and the vitriol oil to carry out two-part leaching extraction, the temperature of one section of acidolysis controls room temperature or 50 ~ 80 DEG C, and the control temperature of reaction of two sections of acidolysis is at 150 ~ 300 DEG C (lower than vitriol oil boiling points 338 DEG C); Effectively the elements such as Ca, Mg, Al, Si are separated with rare earth element simultaneously; The alkali roasting extraction process that comparing appears in the newspapers leads, vitriol oil high temperature extract technology, present invention process realization condition is gentle, technical process realizes extremely easy, the utilising efficiency of hydrochloric acid, sulfuric acid is high, the decomposition leaching yield of rare earth element is higher, rare earth element cost recovery is low, and environment is more friendly, and the rate of recovery of rare earth element can reach more than 95%.
2, the present invention is by the process control of stage extraction, such as residual lanthanum praseodymium element in one section of filter residue of keeping under strict control in a segment unit, avoid the mutual interference between RE element, ensure that the overall rate of recovery of rare earth element on the one hand, ensure that the single and highly purified physical index of rare-earth products simultaneously.
Accompanying drawing explanation
Accompanying drawing is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1:
Get a collection of polishing powder from rare earth waste residue, its composition situation is as following table (dry slag, the dry slag of unit: g/Kg) after testing:
| TREO | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
| 806.2 | 499.6 | 260.4 | 46.2 |
| / | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
| / | 61.97% | 32.30% | 5.73% |
| Ca element (in CaO) | Mg(is in MgO) | Al element is (with Al 2O 3Meter) | Si element is (with SiO 2Meter) |
| 13.4 | 7.8 | 13.1 | 44.5 |
| Obvious impurity (wool pad, foam bits etc.) | |||
| 115.0 |
(1) get a collection of polishing powder from rare earth waste residue (counting 1000Kg after being converted into dry slag), according to the requirement of physical separation, after adding suitable moisture content, isolate obvious impurity.
(2) in above-mentioned polishing powder waste residue, add 900L hydrochloric acid (10mol/L) and carry out an acidolysis, control temperature 60 DEG C, react after 3.5 hours and sample, sample is separated by filtration La, Pr element in rear mensurations filtration filter residue and remains total amount to compare wherein total amount of rare earth be 0.19%; Carry out solid-liquid separation after stopped reaction, obtain one section of leach liquor and one section of filtration filter residue;
Detect one section of leach liquor, main metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element of minute quantity (content is 0.35%);
Filter filter residue to one section to detect, main metal element is wherein Ce, separately has minute quantity La, Pr element remains (accounting comparing total amount of rare earth is 0.19%);
Na is dripped in above-mentioned one section of leach liquor
2sO
4, until no longer there is CaSO in solution
4, MgSO
4obvious sediment thing; Filtering separation removes Ca, Mg element throw out; Adopt NaOH solution to regulate above-mentioned pH of leaching solution to 3.6 again, filtering separation removes Al (OH)
3throw out;
By the filtrate after above-mentioned removal of impurities through extracting and separating, carry out La, Pr and be separated; Again respectively through oxalic acid precipitation, two class rare earth oxide such as lanthanum trioxide and Praseodymium trioxide will be obtained after the ignition of precipitate of rare earth oxalate respectively.
Detect meter heavy, requirement that lanthanum oxide meets " GB/T 4154-2006 lanthanum trioxide ", weight is 253.94Kg, the rate of recovery 97.52%; Requirement that Praseodymium trioxide meets " GB/T 5239-2006 Praseodymium trioxide ", weight is 44.40Kg, the rate of recovery 96.10%.
(3) in gained one section filtration filter residue, add the 700Kg98% vitriol oil and carry out secondary acidolysis, heat-conducting oil heating, 200 DEG C of reactions 5 hours, after being separated by filtration, obtain two sections of leach liquors and two sections of filtration filter residues;
Filter filter residue to two sections to detect, its main component is silicon-dioxide and silicates material, separately has minute quantity rare earth element (content is 1.40%); This solid slag can as the raw materials for production of material of construction or stupalith;
At above-mentioned two sections of leach liquors through oxalic acid precipitation, after the precipitation of rare earth oxalate is carried out high temperature sintering, obtain cerium oxide (IV) respectively.
Detect meter heavy, cerium oxide product meets " GB/T 4155-2012 cerium oxide " requirement, weight 476.92Kg, the rate of recovery 95.46%.
Gather the recovering state of three kinds of rare earth elements such as La, Pr, Ce, the recycled in its entirety rate of polishing powder from rare earth waste residue rare earth elements is 96.16%.
Embodiment 2:
Get a collection of polishing powder from rare earth waste residue, its composition situation is as following table (dry slag, the dry slag of unit: g/Kg) after testing:
| TREO | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
| 856.0 | 643.3 | 172.6 | 46.1 |
| / | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
| / | 75.15% | 20.16% | 4.69% |
| Ca element (in CaO) | Mg(is in MgO) | Al element is (with Al 2O 3Meter) | Si element is (with SiO 2Meter) |
| 10.8 | 5.2 | 12.8 | 33.2 |
| Obvious impurity (wool pad, foam bits etc.) | |||
| 82.0 |
(1) get a collection of polishing powder from rare earth waste residue (counting 1000Kg after being converted into dry slag), according to the requirement of physical separation, after adding suitable moisture content, isolate obvious impurity.
(2) in above-mentioned polishing powder waste residue, add 950L hydrochloric acid (8mol/L) and carry out an acidolysis, control temperature 80 DEG C, react after 4 hours and sample, sample is separated by filtration La, Pr element in rear mensurations filtration filter residue and remains total amount to compare wherein total amount of rare earth be 0.22%; Carry out solid-liquid separation after stopped reaction, obtain one section of leach liquor and one section of filtration filter residue;
Detect one section of leach liquor, main metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element of minute quantity (content is 0.47%);
Filter filter residue to one section to detect, main metal element is wherein Ce, separately has minute quantity La, Pr element remains (accounting comparing total amount of rare earth is 0.22%);
Na is dripped in above-mentioned one section of leach liquor
2sO
4, until no longer there is CaSO in solution
4, MgSO
4obvious sediment thing; Filtering separation removes Ca, Mg element throw out; Adopt NaOH solution to regulate above-mentioned pH of leaching solution to 3.6 again, filtering separation removes Al (OH)
3throw out;
By the filtrate after above-mentioned removal of impurities through extracting and separating, carry out La, Pr and be separated; Obtain lanthanum oxalate and praseodymium oxalate precipitation through oxalic acid precipitation respectively again, oxalic acid solution consumption is no longer to occur that obvious sediment is for reaction end; Two class rare earth oxalate such as lanthanum oxalate and praseodymium oxalate is obtained again after 90 DEG C of dryings.
Detect meter heavy, the purity of lanthanum oxalate (nine water) reaches 99.5%, and weight is 361.92Kg, the rate of recovery 97.10%; The purity of praseodymium oxalate (six water) reaches 99.7%, and weight is 83.94Kg, the rate of recovery 96.02%.
(3) in gained one section filtration filter residue, add the 900Kg98% vitriol oil and carry out secondary acidolysis, heat-conducting oil heating, 220 DEG C of reactions 5 hours, after being separated by filtration, obtain two sections of leach liquors and two sections of filtration filter residues;
Filter filter residue to two sections to detect, its main component is silicon-dioxide and silicates material, separately has minute quantity rare earth element (content is 1.10%); This solid slag can as the raw materials for production of material of construction or stupalith;
At above-mentioned two sections of leach liquors through oxalic acid precipitation, oxalic acid solution consumption is no longer to occur that obvious sediment is for reaction end; Sedemesis (III) is obtained again after 90 DEG C of dryings.
Detect meter heavy, the purity of Sedemesis (nine water) reaches 99.5% requirement, weight 1263.45Kg, the rate of recovery 95.70%.
Gather the recovering state of three kinds of rare earth elements such as La, Pr, Ce, the recycled in its entirety rate of polishing powder from rare earth waste residue rare earth elements is 96.12%.
Claims (4)
1. the method for sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue, is characterized in that the method comprises the following steps:
(1) polishing powder from rare earth waste residue is carried out physical separation, remove foreign material;
(2) one segment units: the hydrochloric acid adding 5 ~ 12mol/L in polishing powder waste residue carries out an acidolysis, control temperature is room temperature or 50 ~ 80 DEG C, obtains being rich in one section of leach liquor of La, Pr element and being rich in one section of filter residue of Ce element after being separated by filtration; The add-on of hydrochloric acid is determined by the content situation of La, Pr, Ca, Mg, Al element in waste residue, all form 1.1 ~ 2.5 times of muriatic theoretical demand molar weight by above-mentioned element and add hydrochloric acid, react and compare one section of filter residue rare earth element total amount with lanthanum praseodymium element residual in one section of filter residue and be less than 0.3% for terminal; In one section of leach liquor, add the salt of containing sulfate radicals, being separated and removing Ca, Mg element throw out, no longer there is CaSO in the add-on of the salt of containing sulfate radicals
4, MgSO
4white precipitate be terminal; Regulate the pH value of one section of leach liquor to 3 ~ 4.5 by alkali again, be separated and remove Al element throw out; For section removal of impurities liquid of after above-mentioned removal of impurities, one of following method is adopted to obtain rare earth compound corresponding to La and Pr element:
Method one: obtain lanthanum oxalate and praseodymium oxalate after extracting and separating, oxalic acid precipitation, drying;
Method two: obtain lanthanum oxalate praseodymium after oxalic acid precipitation, drying;
Method three: obtain lanthanum trioxide and Praseodymium trioxide after extracting and separating, precipitation, calcination;
Method four: obtain lanthanum praseodymium oxide after precipitation, calcination;
(3) two segment units: add the vitriol oil and carry out secondary acidolysis in the one section of filter residue being rich in Ce, control temperature of reaction at 150 ~ 300 DEG C, in 2 ~ 8 hours reaction times, obtain two sections of leach liquors and two sections of filter residues after being separated by filtration; The add-on of the vitriol oil is determined by Ce content in one section of filter residue, by CeO in one section of filter residue
21.1 ~ 1.6 times that are all converted into the theoretical demand molar weight of ceric sulfate add the vitriol oil; For above-mentioned two sections of leach liquors, one of following method is adopted to obtain rare earth compound corresponding to Ce element:
Method five: obtain Sedemesis after oxalic acid precipitation, drying;
Method six: obtain cerium oxide after precipitation, high-temperature calcination.
2. the method for a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue according to claim 1, is characterized in that: described polishing powder from rare earth waste residue refers to the polishing powder waste residue of the total amount of the rare earth oxide after for liquid crystal display, opticglass, stone material, Crystal ornaments polishing at more than 10wt%.
3. the method for a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue according to claim 1, is characterized in that: the salt of step (2) described containing sulfate radicals is the one in sodium sulfate, potassium sulfate, ammonium sulfate; Described alkali is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
4. the method for a kind of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue according to claim 1, is characterized in that: the vitriol oil described in step (3) to be massfraction be 98% the vitriol oil.
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| CN104946895B (en) * | 2015-06-29 | 2017-04-26 | 包头市新世纪稀土有限责任公司 | Rare earth compound recycling method utilizing waste rare earth polishing powder |
| CN105039729A (en) * | 2015-08-30 | 2015-11-11 | 常州思宇环保材料科技有限公司 | Method for recycling rare earth oxide from rare earth optical glass waste residues |
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| CN108531735B (en) * | 2018-04-23 | 2020-03-31 | 湖南稀土金属材料研究院 | Method for extracting rare earth oxide from polishing powder waste |
| CN108559851B (en) * | 2018-06-22 | 2023-11-17 | 长沙中硅环保科技有限公司 | System and method for cooperatively disposing rare earth polishing powder waste by cement kiln |
| CN108950251B (en) * | 2018-08-01 | 2021-08-24 | 连云港高品再生资源有限公司 | Method for recovering rare earth elements |
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| CN114381206B (en) * | 2022-01-07 | 2023-04-14 | 甘肃金阳高科技材料有限公司 | Method for preparing rare earth polishing powder by regenerating glass polishing waste residues |
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| CN103103361A (en) * | 2013-02-28 | 2013-05-15 | 包头稀土研究院 | Method for preparing rare earth oxide from rare earth polishing powder waste |
| CN103305697A (en) * | 2013-06-13 | 2013-09-18 | 蓝思科技股份有限公司 | Recovering and reutilizing method of waste residues and waste liquid of rare earth polishing powder |
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