CN104060111A - Method for performing clear segmented recycling on rare earth elements from rare earth polishing powder waste residues - Google Patents
Method for performing clear segmented recycling on rare earth elements from rare earth polishing powder waste residues Download PDFInfo
- Publication number
- CN104060111A CN104060111A CN201410329931.6A CN201410329931A CN104060111A CN 104060111 A CN104060111 A CN 104060111A CN 201410329931 A CN201410329931 A CN 201410329931A CN 104060111 A CN104060111 A CN 104060111A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- polishing powder
- section
- waste residue
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for performing clear segmented recycling on rare earth elements from rare earth polishing powder waste residues. The method comprises the following steps: by utilizing the technical scheme of segmented extraction, sorting the components aiming at ineffective polishing powder particles in the polishing powder waste residues, extracting elements La and Pr from the ineffective polishing powder particles in a first section of the link, and extracting element Ce from the ineffective polishing powder particles in a second section of the link; realizing rare earth metal clear separation and recovery based on the two-section process flow; and respectively removing the impurity components and impurity elements in the waste residues on different process sections through a chemical method, so that high physical indexes of the product are ensured. The invention provides a method through which the resource efficiency is high, the process condition is mild, the process flow is simple and convenient and the product accords with the high physical indexes.
Description
Technical field
The present invention relates to a kind of from polishing powder from rare earth waste residue the method for recovering rare earth element, belong to the technical field of waste resource comprehensive utilization.
Background technology
Polishing powder from rare earth, because of its unique physics, chemical property and good 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, advantage that planeness is high is widely used in the polishing of the glass substrate of optical lens, liquid-crystal display, panel computer, mobile phone faceplate, making hard disk.Approximately 15 of the Large-scale enterprises that at present domestic existing cerium base polishing powder from rare earth is produced, approximately 1.6 ten thousand tons of yearly capacities, 1.4 ten thousand tons of actual consumption rare earths above (REO).According to the analytic statistics to main polishing powder from rare earth product 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%.
Polishing powder from rare earth in use often first water want furnishing slurries, 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 of polishing (as glass, stone material etc.) is also along with polishing process constantly in enrichment in slurries system.Because production technique reason, above-mentioned cerium base polishing powder from rare earth finally all inevitably becomes a class trade waste in polishing use procedure, after press filtration, collects 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 base polishing powder from rare earth particle 1) losing efficacy; 2) throw the base material chip chipping away, as glass micro mist, stone material chip etc.; 3) derive from thing under the throwing of polishing pad, 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 Rare-earth Mine mineral products resource of required consumption can get more and more on the one hand, on the other hand, the polishing powder from rare earth waste residue that in use formed is 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, from polishing powder from rare earth waste residue, carry out the extraction of rare earth element and reclaim, 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 that 201310233211.5) discloses fail rare earth polishing powder, the method is by the physical chemistry processing 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 is used.Applicant is at " a kind of devices and methods therefor of 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 method that realizes useless polishing powder from rare earth and clean 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.Domestic patent " a kind of method by useless rare earth abrasive substance recovering rare earth element " (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 Waste gurry ratio is also quite large.Domestic patent " a kind of method of producing lanthanum oxalate cerium from polishing powder from rare earth waste residue " (patent No.: 201210155031.5) thus adopt the vitriol oil to leach processing recovering rare earth element to waste residue, in actual application, have that process costs is higher, vitriol oil consumption is bigger than normal, product cannot be guaranteed the limitation such as purity requirement.Domestic patent " a kind of method of 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, Waste gurry ratio is large.Therefore, more economy, Production Flow Chart are more easy to invent a kind of manufacturing process, have more on the whole the novel method that industrial technology is worth, to promoting the industrialization technology level 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 all deficiencies for existing polishing powder from rare earth rare earth elements recovery technology, a kind of method that resource efficiency is high, processing condition are gentle, technical process is easy, product meets high physical index is provided.Inventor herein conducts in-depth research, the technical scheme that discovery utilizes 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, can realize rare earth element sharpening Separation and Recovery simultaneously; And remove respectively impurity component and the impurity element in waste residue by chemical process at different process sections, thereby guarantee the high physical index of product.The advantageous effects of comprehensive above-mentioned several respects, thus the present invention completed.
In order more clearly to explain technical scheme of the present invention, 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 analysis to glossing and polishing process, can understand polishing powder from rare earth waste residue component complexity, all kinds of component things and characteristic situation thereof are described as follows:
1) the cerium base polishing powder from rare earth particle losing 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 of polishing powder from rare earth composition 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) throw the base material chip chipping away, as glass micro mist, stone material chip etc.; Main component is SiO
2and silicate glass, calcium carbonate, and calcium, magnesium oxide;
3) derive from thing under the throwing of polishing pad, 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 from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that the method comprises the following steps:
(1) polishing powder from rare earth waste residue is carried out to physical separation, remove foreign material;
(2) one segment units: add the hydrochloric acid of 5～12mol/L to carry out an acidolysis in polishing powder waste residue, controlling temperature is room temperature or 50～80 DEG C, the one section of filter residue that obtains being rich in one section of leach liquor of La, Pr element after being separated by filtration and be rich in Ce element; The add-on of hydrochloric acid is determined by the content situation of La, Pr, Ca, Mg, Al element in waste residue, all forming muriatic theory by above-mentioned element needs 1.1～2.5 times of molar weight to add hydrochloric acid, and reaction is compared one section of filter residue rare earth element total amount taking residual lanthanum praseodymium element in one section of filter residue and is less than 0.3% as terminal; In one section of leach liquor, adding the salt of containing sulfate radicals, separate and remove 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 again pH value to 3～4.5 of one section of leach liquor by alkali, separate and remove Al element throw out; For one section of removal of impurities liquid after above-mentioned removal of impurities, adopt one of following method to obtain La and rare earth compound corresponding to Pr element:
Method one: obtain lanthanum oxalate and praseodymium oxalate through extracting and separating, oxalic acid precipitation, after dry;
Method two: obtain lanthanum oxalate praseodymium through oxalic acid precipitation, after dry;
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 to carry out secondary acidolysis in the one section of filter residue that is 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
2the theory that is all converted into ceric sulfate needs 1.1～1.6 times of molar weight to add the vitriol oil; For above-mentioned two sections of leach liquors, adopt one of following method to obtain the rare earth compound that Ce element is corresponding:
Method five: obtain Sedemesis through oxalic acid precipitation, after dry;
Method six: obtain cerium oxide after precipitation, high-temperature calcination.
Below invention is described further:
Of the present invention a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: described polishing powder from rare earth waste residue refers to the polishing powder waste residue more than 10wt% for the total amount of the rare earth oxide after liquid crystal display, opticglass, stone material, Crystal ornaments polishing.
Of the present invention a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: the salt of the described containing sulfate radicals of step (2) is the one in sodium sulfate, potassium sulfate, ammonium sulfate; Described alkali is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
Of the present invention a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: the vitriol oil described in step (3) is that massfraction is 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, carry out respectively an acidolysis, secondary acidolysis by hydrochloric acid, the vitriol oil and reach the technical object that rare earth element segmentation is leached, can effectively 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, separate thereby complete sharpening between La, Pr and Ce element.
On the basis of 2, leaching in segmentation, dispose by the removal of impurities to leach liquor, avoided the quality influence of element to rare-earth products such as Ca, Mg, Al, guarantee 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 to use the acid larger to environmental hazard such as HF acid, nitric acid, leach extraction but adopt hydrochloric acid and the vitriol oil to carry out two-part, the temperature of one section of acidolysis is controlled at 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 338 DEG C of vitriol oil boiling points); Effectively the elements such as Ca, Mg, Al, Si are separated with rare earth element simultaneously; Alkali roasting extraction process, vitriol oil high temperature extract technology that comparing appears in the newspapers leads, technique realization condition gentleness of the present invention, 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 the one section of filter residue of keeping under strict control in a segment unit, avoid the phase mutual interference between RE element, guaranteed on the one hand the overall rate of recovery of rare earth element, guaranteed the single and highly purified physical index of rare-earth products simultaneously.
brief description of the drawings
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, add after suitable moisture content, isolate obvious impurity.
(2) in above-mentioned polishing powder waste residue, add 900L hydrochloric acid (10mol/L) to carry out an acidolysis, control temperature 60 C, react after 3.5 hours sampling, sample is separated by filtration rear mensuration and filters in filter residue La, the residual total amount of Pr element to compare wherein total amount of rare earth be 0.19%; After stopped reaction, carry out solid-liquid separation, obtain one section of leach liquor and one section of filtration filter residue;
One section of leach liquor is detected, and major metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element (content is 0.35%) of minute quantity;
Filter filter residue to one section and detect, major metal element is wherein Ce, separately has minute quantity La, Pr element residual (accounting of comparing total amount of rare earth is 0.19%);
In above-mentioned one section of leach liquor, drip Na
2sO
4, until no longer there is CaSO in solution
4, MgSO
4obvious sediment thing; Filtering separation is removed Ca, Mg element throw out; Adopt NaOH solution to regulate above-mentioned pH of leaching solution to 3.6, filtering separation is removed Al (OH) again
3throw out;
Filtrate after above-mentioned removal of impurities, through extracting and separating, is carried out to La, Pr and separated; Respectively through oxalic acid precipitation, the two class rare earth oxides such as lanthanum trioxide and Praseodymium trioxide will be obtained respectively after the ignition of precipitate of rare earth oxalate again.
Detect meter heavy, lanthanum oxide meets " GB/T 4154-2006 lanthanum trioxide " requirement, and weight is 253.94Kg, the rate of recovery 97.52%; Praseodymium trioxide meets " GB/T 5239-2006 Praseodymium trioxide " requirement, and weight is 44.40Kg, the rate of recovery 96.10%.
(3) in one section of gained filters filter residue, add the 700Kg98% vitriol oil to carry out secondary acidolysis, heat-conducting oil heating, 200 DEG C of reactions 5 hours, obtains two sections of leach liquors and two sections of filtration filter residues after being separated by filtration;
Filter filter residue to two sections and 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 be used as the raw materials for production of material of construction or stupalith;
, through oxalic acid precipitation the precipitation of rare earth oxalate is carried out obtaining respectively cerium oxide (IV) after high temperature sintering at above-mentioned two sections of leach liquors.
Detect meter heavy, cerium oxide product meets " GB/T 4155-2012 cerium oxide " requirement, weight 476.92Kg, the rate of recovery 95.46%.
The recovering state that gathers 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, add after suitable moisture content, isolate obvious impurity.
(2) in above-mentioned polishing powder waste residue, add 950L hydrochloric acid (8mol/L) to carry out an acidolysis, control 80 DEG C of temperature, react after 4 hours sampling, sample is separated by filtration rear mensuration and filters in filter residue La, the residual total amount of Pr element to compare wherein total amount of rare earth be 0.22%; After stopped reaction, carry out solid-liquid separation, obtain one section of leach liquor and one section of filtration filter residue;
One section of leach liquor is detected, and major metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element (content is 0.47%) of minute quantity;
Filter filter residue to one section and detect, major metal element is wherein Ce, separately has minute quantity La, Pr element residual (accounting of comparing total amount of rare earth is 0.22%);
In above-mentioned one section of leach liquor, drip Na
2sO
4, until no longer there is CaSO in solution
4, MgSO
4obvious sediment thing; Filtering separation is removed Ca, Mg element throw out; Adopt NaOH solution to regulate above-mentioned pH of leaching solution to 3.6, filtering separation is removed Al (OH) again
3throw out;
Filtrate after above-mentioned removal of impurities, through extracting and separating, is carried out to La, Pr and 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 as reaction end; After 90 DEG C are dried, obtain the two class rare earth oxalates such as lanthanum oxalate and praseodymium oxalate again.
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 one section of gained filters filter residue, add the 900Kg98% vitriol oil to carry out secondary acidolysis, heat-conducting oil heating, 220 DEG C of reactions 5 hours, obtains two sections of leach liquors and two sections of filtration filter residues after being separated by filtration;
Filter filter residue to two sections and 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 be used 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 as reaction end; After 90 DEG C are dried, obtain Sedemesis (III) again.
Detect meter heavy, the purity of Sedemesis (nine water) reaches 99.5% requirement, weight 1263.45Kg, the rate of recovery 95.70%.
The recovering state that gathers 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. a 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 to physical separation, remove foreign material;
(2) one segment units: add the hydrochloric acid of 5～12mol/L to carry out an acidolysis in polishing powder waste residue, controlling temperature is room temperature or 50～80 DEG C, the one section of filter residue that obtains being rich in one section of leach liquor of La, Pr element after being separated by filtration and be rich in Ce element; The add-on of hydrochloric acid is determined by the content situation of La, Pr, Ca, Mg, Al element in waste residue, all forming muriatic theory by above-mentioned element needs 1.1～2.5 times of molar weight to add hydrochloric acid, and reaction is compared one section of filter residue rare earth element total amount taking residual lanthanum praseodymium element in one section of filter residue and is less than 0.3% as terminal; In one section of leach liquor, adding the salt of containing sulfate radicals, separate and remove 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 again pH value to 3～4.5 of one section of leach liquor by alkali, separate and remove Al element throw out; For one section of removal of impurities liquid after above-mentioned removal of impurities, adopt one of following method to obtain La and rare earth compound corresponding to Pr element:
Method one: obtain lanthanum oxalate and praseodymium oxalate through extracting and separating, oxalic acid precipitation, after dry;
Method two: obtain lanthanum oxalate praseodymium through oxalic acid precipitation, after dry;
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 to carry out secondary acidolysis in the one section of filter residue that is 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
2the theory that is all converted into ceric sulfate needs 1.1～1.6 times of molar weight to add the vitriol oil; For above-mentioned two sections of leach liquors, adopt one of following method to obtain the rare earth compound that Ce element is corresponding:
Method five: obtain Sedemesis through oxalic acid precipitation, after dry;
Method six: obtain cerium oxide after precipitation, high-temperature calcination.
According to claim 1 a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: described polishing powder from rare earth waste residue refers to the polishing powder waste residue more than 10wt% for the total amount of the rare earth oxide after liquid crystal display, opticglass, stone material, Crystal ornaments polishing.
According to claim 1 a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: the salt of the described containing sulfate radicals of step (2) is the one in sodium sulfate, potassium sulfate, ammonium sulfate; Described alkali is the one in sodium hydroxide, potassium hydroxide, ammoniacal liquor.
According to claim 1 a kind of from polishing powder from rare earth waste residue the method for sharpening segmentation recovering rare earth element, it is characterized in that: the vitriol oil described in step (3) is that massfraction is 98% the vitriol oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410329931.6A CN104060111B (en) | 2014-07-12 | 2014-07-12 | A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410329931.6A CN104060111B (en) | 2014-07-12 | 2014-07-12 | A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104060111A true CN104060111A (en) | 2014-09-24 |
| CN104060111B CN104060111B (en) | 2015-09-02 |
Family
ID=51548040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410329931.6A Active CN104060111B (en) | 2014-07-12 | 2014-07-12 | A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104060111B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946895A (en) * | 2015-06-29 | 2015-09-30 | 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 |
| CN107083496A (en) * | 2017-04-19 | 2017-08-22 | 乐山东承新材料有限公司 | A kind of method that rare earth oxide is extracted from rare earth waste |
| CN108531735A (en) * | 2018-04-23 | 2018-09-14 | 湖南稀土金属材料研究院 | The method of Extraction of rare earth oxide from polishing powder waste material |
| CN108559851A (en) * | 2018-06-22 | 2018-09-21 | 长沙中硅水泥技术开发有限公司 | A kind of System and method for of cement kiln synergic processing polishing powder from rare earth waste material |
| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
| CN110241309A (en) * | 2019-05-08 | 2019-09-17 | 湖南景翌湘台环保高新技术开发有限公司 | A kind of method that useless polishing powder from rare earth extracts white carbon black and rare earth water purification agent |
| CN112322915A (en) * | 2020-11-23 | 2021-02-05 | 湖北沛丰生物科技股份有限公司 | Method for recycling polished broken rice flour |
| CN114381206A (en) * | 2022-01-07 | 2022-04-22 | 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115822A (en) * | 2010-11-18 | 2011-07-06 | 吴泉锦 | Method for recovering rare earth oxide from fluorescent powder and polishing powder waste |
| 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 |
| 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 |
-
2014
- 2014-07-12 CN CN201410329931.6A patent/CN104060111B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115822A (en) * | 2010-11-18 | 2011-07-06 | 吴泉锦 | Method for recovering rare earth oxide from fluorescent powder and polishing powder waste |
| 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 |
| 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 |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946895A (en) * | 2015-06-29 | 2015-09-30 | 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 |
| CN107083496A (en) * | 2017-04-19 | 2017-08-22 | 乐山东承新材料有限公司 | A kind of method that rare earth oxide is extracted from rare earth waste |
| CN108531735A (en) * | 2018-04-23 | 2018-09-14 | 湖南稀土金属材料研究院 | The method of Extraction of rare earth oxide from polishing powder waste material |
| 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 |
| CN108559851A (en) * | 2018-06-22 | 2018-09-21 | 长沙中硅水泥技术开发有限公司 | A kind of System and method for of cement kiln synergic processing polishing powder from rare earth waste material |
| 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 |
| CN108950251A (en) * | 2018-08-01 | 2018-12-07 | 连云港高品再生资源有限公司 | The recovery method of rare earth element |
| CN110241309A (en) * | 2019-05-08 | 2019-09-17 | 湖南景翌湘台环保高新技术开发有限公司 | A kind of method that useless polishing powder from rare earth extracts white carbon black and rare earth water purification agent |
| 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 |
| CN112322915A (en) * | 2020-11-23 | 2021-02-05 | 湖北沛丰生物科技股份有限公司 | Method for recycling polished broken rice flour |
| CN114381206A (en) * | 2022-01-07 | 2022-04-22 | 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104060111B (en) | 2015-09-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104060111B (en) | A kind of method of sharpening segmentation recovering rare earth element from polishing powder from rare earth waste residue | |
| CN104087757B (en) | A kind of easy method of recovering rare earth element from polishing powder from rare earth waste residue | |
| CN102145905B (en) | Method for preparing metallurgy-level aluminum oxide by using fluidized bed pulverized fuel ash | |
| CN100413981C (en) | Method for extracting aluminum from high-silicon aluminum-containing mineral raw material by acid process | |
| CN102515213A (en) | Integrated utilization method of low grade magnesite | |
| US11066723B2 (en) | Systems and methods to chemically treat metal-bearing waste streams to recover value-added materials | |
| CN104386720B (en) | Method for acid-alkali combined extraction of alumina from high-silicon aluminum-containing mineral raw material | |
| CN104711424B (en) | A kind of method of recovering rare earth and aluminium in removal of impurities slag from weathered superficial leaching rare-earth ore leachate | |
| WO2022116870A1 (en) | Method for recovering rare earths from waste cerium-based rare-earth polishing powder by two-step acid leaching stepwise separation | |
| CN101463426A (en) | Comprehensive utilization method for red mud | |
| CN103589872A (en) | Method for recovering titanium from red mud slag | |
| CN103193213A (en) | Method for comprehensively utilizing low-grade phosphate ores | |
| CN102659559B (en) | Method for preparing lanthanum cerium oxalate from rare earth polishing powder waste residue | |
| CN106747497A (en) | The method for preparing corundum-mullite composite diphase material | |
| CN102417978A (en) | Method for enriching titanium in coal gangue | |
| CN103349994A (en) | Method for recovering catalyst and separating aluminum-containing compound from coal ash | |
| CN100336921C (en) | Method for extracting aluminium and iron from high-iron bauxite trihydrate | |
| CN101798095B (en) | Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock | |
| CN106629743B (en) | A method of ceramic glaze quartz sand is produced using quartz tail sand | |
| CN110482582A (en) | Method that is a kind of while extracting aluminium oxide in flyash and red mud | |
| CN100357462C (en) | Method for comprehensively utilizing serpentine resource | |
| CN103215439A (en) | Method for extracting scandium from scandium enrichment | |
| CN101899581A (en) | Method for preparing metal magnesium and boron-enriched material from ascharite serving as raw material by vacuum thermal reduction method | |
| CN103589871A (en) | Method for recovering aluminum from red mud slag | |
| CN103738989B (en) | A kind of middle-low bauxite produces the method for aluminum oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |