CN104087757B - A kind of easy method of recovering rare earth element from polishing powder from rare earth waste residue - Google Patents
A kind of easy method of 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 easy method of recovering rare earth element from polishing powder from rare earth waste residue, utilizes first to carry out excellent molten acidolysis, carry out alkali again and dissolve and wash away de-technical scheme and can realize component sorting for the inefficacy polishing powder particle in polishing powder waste residue; From inefficacy polishing powder particle, extract La, Pr element in excellent molten acidolysis link, the filtration filter residue after extracting is carried out to alkali again and dissolves and washes away de-, the Si element in degree of depth removal system thus recovering rare earth Ce element; Whole technological process is very easy.The rare earth number of dropouts of present invention process process is little, and the rate of recovery of rare earth element can reach more than 96%; Under the processing condition of gentleness, raw material energy consumption has higher utilising efficiency; Therefore, the technology of the present invention has remarkable cost advantage; There is higher technique simultaneously and clean level.
Description
Technical field
The present invention relates to a kind of easy 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, invent a kind of technique more easy, full recovering rare earth element novel method that processing condition are more gentle, 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 all deficiencies for existing polishing powder from rare earth rare earth elements recovery technology, provide that a kind of technical process is easy, processing condition are gentle, the method that rare earth element newly reclaims can be realized.Inventor herein conducts in-depth research, and finds to utilize first to carry out excellent molten acidolysis, carry out alkali again and dissolve and wash away de-technical scheme and can realize component sorting for the inefficacy polishing powder particle in polishing powder waste residue; From inefficacy polishing powder particle, extract La, Pr element in excellent molten acidolysis link, the filtration filter residue after extracting is carried out to alkali again and dissolves and washes away de-, the Si element in degree of depth removal system thus collect highly purified Rare-Earth Ce element; Based on the technical process of above-mentioned easy, while realizing the excellent molten separation of rare earth element, remove impurity component in waste residue and impurity element by chemical process respectively at different process sections, thus reach the technical purpose of purifying rare earth element.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 easy method of 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) hydrochloric acid adding 5 ~ 12mol/L in polishing powder waste residue carries out excellent molten acidolysis, and control temperature is room temperature or 50 ~ 80 DEG C, obtains being rich in the excellent molten leach liquor of La, Pr element and being rich in the excellent lixiviation slag 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 excellent lixiviation slag rare earth element total amount with lanthanum praseodymium element residual in excellent lixiviation slag and be less than 0.5% for terminal; In excellent molten 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 excellent molten leach liquor to 3 ~ 4.5 by alkali again, be separated and remove Al element throw out; For the excellent molten removal of impurities liquid after above-mentioned removal of impurities, one of following method is adopted to obtain rare earth oxide corresponding to La and Pr element:
Method one: obtain lanthanum trioxide and Praseodymium trioxide after extracting and separating, precipitation, calcination;
Method two: obtain lanthanum praseodymium oxide after precipitation, calcination;
(3) in the excellent lixiviation slag being rich in Ce, add sodium hydroxide, post-heating of sizing mixing, to 100 ~ 200 DEG C, reacts discharging after 2 ~ 8 hours; Sodium hydroxide concentration is determined by the content situation of Si element in excellent lixiviation slag, and all form the theoretical demand molar weight of silicate by Si element 1.1 ~ 2 times add sodium hydroxide; Material water carries out wash-out and collects the molten elutriant of alkali; Wash-out residuum is carried out drying, obtains cerium oxide.
Below invention is described further:
The easy method of a kind of 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 easy method of a kind of 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 easy method of a kind of recovering rare earth element from polishing powder from rare earth waste residue of the present invention, is characterized in that: sodium hydroxide described in step (3) is sodium hydrate solid or 30% sodium hydroxide solution.
The easy method of a kind of recovering rare earth element from polishing powder from rare earth waste residue of the present invention, is characterized in that: described in step (3), the main component of the molten elutriant of alkali is Na
2siO
3, as water glass or water glass raw materials for production.
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, excellent molten acidolysis is carried out by hydrochloric acid, by La(III), Pr(III) extract in excellent molten leach liquor, and Ce (IV) is resided in excellent lixiviation slag.
2, for the excellent molten leach liquor being rich in La, Pr element, removed Ca, Mg, Al element of system by chemical process, and obtain La, Pr element chlorated liquid of purifying, and then the rare-earth products of La, Pr element can be further converted to.
3, for the excellent lixiviation slag being rich in Ce, dissolve and wash away de-method by alkali and remove Si element in system, and obtain Ce (IV) the element product of purifying.
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, there is not the process procedure using the vitriol oil to carry out high temperature leaching, there is not alkali fusion roasting (temperature general requirement is more than 500 DEG C); But the leaching only using hydrochloric acid to carry out excellent dissolubility matter is extracted, excellent molten acidolysis reaction condition is extremely gentle, be aided with and comprise that alkali is molten is eluted in interior chemical subtraction means, remove Ca, Mg, Al element in leach liquor, remove the Si element in excellent molten residue, thus reaching the technical purpose of recovering rare earth element, whole technological process is very easy.
2, the rare earth number of dropouts of present invention process process is little, and the rate of recovery of rare earth element can reach more than 96%; Under the processing condition of gentleness, raw material energy consumption has higher utilising efficiency; Therefore, the technology of the present invention has remarkable cost advantage; There is higher technique simultaneously and clean level.
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 |
815.6 | 580.7 | 188.7 | 46.2 |
/ | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
/ | 71.20% | 23.14% | 5.66% |
Ca element (in CaO) | Mg(is in MgO) | Al element is (with Al 2O 3Meter) | Si element is (with SiO 2Meter) |
11.4 | 6.2 | 12.0 | 47.4 |
Obvious impurity (wool pad, foam bits etc.) | |||
107.4 |
(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 (10mol/L) and carry out excellent molten acidolysis, control temperature 60 DEG C, react after 3 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 0.30%; Carry out solid-liquid separation after stopped reaction, obtain excellent molten leach liquor and excellent lixiviation slag;
Detect excellent molten leach liquor, main metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element of minute quantity (content is 0.18%);
Detect excellent lixiviation slag, main metal element is wherein Ce, separately has minute quantity La, Pr element remains (accounting comparing total amount of rare earth is 0.30%);
Na is dripped in above-mentioned excellent molten 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/T4154-2006 lanthanum trioxide ", weight is 182.66Kg, the rate of recovery 96.80%; Requirement that Praseodymium trioxide meets " GB/T5239-2006 Praseodymium trioxide ", weight is 44.89Kg, the rate of recovery 97.16%.
(3) in the excellent lixiviation slag of gained, 290Kg30% sodium hydroxide solution is added, 120 DEG C of reactions 3 hours, discharging after cooling; Material clear water washs 3 times, collects elutriant; Wash-out residuum, after 120 DEG C of dryings, obtains cerium oxide (IV).
After testing, elutriant main component is water glass, as water glass or water glass raw materials for production.
Detect meter heavy, cerium oxide product meets " GB/T4155-2012 cerium oxide " requirement, weight 560.96Kg, the rate of recovery 96.60%.
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 96.68%.
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 |
842.3 | 618.6 | 187.5 | 36.2 |
/ | CeO 2/TREO | La 2O 3/TREO | Pr 6O 11/TREO |
/ | 73.44% | 22.26% | 4.30% |
Ca element (in CaO) | Mg(is in MgO) | Al element is (with Al 2O 3Meter) | Si element is (with SiO 2Meter) |
11.8 | 4.2 | 10.3 | 41.0 |
Obvious impurity (wool pad, foam bits etc.) | |||
90.4 |
(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 1000L hydrochloric acid (8mol/L) and carry out excellent molten acidolysis, control temperature 70 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 0.25%; Carry out solid-liquid separation after stopped reaction, obtain excellent molten leach liquor and excellent lixiviation slag;
Detect excellent molten leach liquor, main metal element is wherein La, Pr, Ca, Mg, Al, separately has the Ce element of minute quantity (content is 0.12%);
Detect excellent lixiviation slag, main metal element is wherein Ce, separately has minute quantity La, Pr element remains (accounting comparing total amount of rare earth is 0.25%);
Na is dripped in above-mentioned excellent molten 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 oxalic acid precipitation, obtain lanthanum praseodymium oxide respectively by after the ignition of precipitate of rare earth oxalate.
Detect meter heavy, lanthanum praseodymium oxide TREO=99.5%, (La
2o
3+ Pr
6o
11)/TREO=99.1%, weight is 215.83Kg, the rate of recovery 96.48%.
(3) in the excellent lixiviation slag of gained, 250Kg30% sodium hydroxide solution is added, 110 DEG C of reactions 4 hours, discharging after cooling; Material clear water washs 4 times, collects elutriant; Wash-out residuum, after 120 DEG C of dryings, obtains cerium oxide (IV).
After testing, elutriant main component is water glass, as water glass or water glass raw materials for production.
Detect meter heavy, cerium oxide product meets " GB/T4155-2012 cerium oxide " requirement, weight 590.95Kg, the rate of recovery 96.50%.
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 96.49%.
Claims (5)
1. the easy method of 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) hydrochloric acid adding 5 ~ 12mol/L in polishing powder waste residue carries out excellent molten acidolysis, and control temperature is room temperature or 50 ~ 80 DEG C, obtains being rich in the excellent molten leach liquor of La, Pr element and being rich in the excellent lixiviation slag 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 excellent lixiviation slag rare earth element total amount with lanthanum praseodymium element residual in excellent lixiviation slag and be less than 0.5% for terminal; In excellent molten 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 excellent molten leach liquor to 3 ~ 4.5 by alkali again, be separated and remove Al element throw out; For the excellent molten removal of impurities liquid after above-mentioned removal of impurities, one of following method is adopted to obtain rare earth oxide corresponding to La and Pr element:
Method one: obtain lanthanum trioxide and Praseodymium trioxide after extracting and separating, precipitation, calcination;
Method two: obtain lanthanum praseodymium oxide after precipitation, calcination;
(3) in the excellent lixiviation slag being rich in Ce, add sodium hydroxide, post-heating of sizing mixing, to 100 ~ 200 DEG C, reacts discharging after 2 ~ 8 hours; Sodium hydroxide concentration is determined by the content situation of Si element in excellent lixiviation slag, and all form the theoretical demand molar weight of silicate by Si element 1.1 ~ 2 times add sodium hydroxide; Material water carries out wash-out and collects the molten elutriant of alkali; Wash-out residuum is carried out drying, obtains cerium oxide.
2. the easy method of a kind of 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 easy method of a kind of 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 easy method of a kind of recovering rare earth element from polishing powder from rare earth waste residue according to claim 1, is characterized in that: sodium hydroxide described in step (3) is sodium hydrate solid or 30% sodium hydroxide solution.
5. the easy method of a kind of recovering rare earth element from polishing powder from rare earth waste residue according to claim 1, is characterized in that: described in step (3), the main component of the molten elutriant of alkali is Na
2siO
3, as water glass or water glass raw materials for production.
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CN106319218B (en) * | 2015-06-16 | 2019-12-24 | 有研稀土新材料股份有限公司 | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum-silicon waste |
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 |
CN109999531B (en) * | 2019-02-28 | 2021-06-15 | 宜兴新乐祺纺织印染有限公司 | Production method of low-radioactivity negative ion nano material |
TWI738565B (en) * | 2020-11-13 | 2021-09-01 | 國立臺北科技大學 | Method for recovery and reuse of glass polishing waste |
CN112725623B (en) | 2020-12-02 | 2022-09-09 | 北京工业大学 | Method for separating and extracting rare earth and regenerated rare earth polishing powder from waste rare earth polishing powder |
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 |
CN114700180B (en) * | 2022-03-21 | 2023-06-20 | 中南大学 | Method for recycling rare earth components in waste polishing powder |
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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 |
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