CN106498189B - A kind of recovery method of discarded polishing powder from rare earth - Google Patents

A kind of recovery method of discarded polishing powder from rare earth Download PDF

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CN106498189B
CN106498189B CN201610932244.2A CN201610932244A CN106498189B CN 106498189 B CN106498189 B CN 106498189B CN 201610932244 A CN201610932244 A CN 201610932244A CN 106498189 B CN106498189 B CN 106498189B
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rare earth
polishing powder
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discarded polishing
lead
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CN106498189A (en
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史培阳
王希鑫
丁文清
李鑫哲
赵化源
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/32—Alkali metal silicates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • 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

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
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  • Mechanical Engineering (AREA)
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  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：By proportioning, discarded polishing powder from rare earth, reducing agent and highly basic are weighed, after mixing, 60~240min of reduction reaction is carried out at 600~800 DEG C, obtains reduzate；By reduzate water quenching to room temperature, cooled product is obtained；Cooled product is subjected to rotary filter press, obtains the mixture and metallic lead of rich rare earth material and aqueous silicate solution；The mixture of aqueous silicate solution and rich rare earth material obtains aqueous silicate solution and rich rare earth material by filtering.The present invention solves pollution of the lead element to environment in discarded polishing powder from rare earth, valuable constituent element rare earth, lead and element silicon recycling in discarded polishing powder from rare earth are realized simultaneously, lead content can be neglected in rich rare earth material after the art of this patent is handled, rich rare earth material Leaching Heavy Metals meet national standard, the innoxious of discarded polishing powder from rare earth, minimizing and recycling treatment are realized, meets the target that China develops a circular economy with energy-saving and emission-reduction.

Description

A kind of recovery method of discarded polishing powder from rare earth
Technical field：
The invention belongs to dangerous field of solid waste treating technology, and in particular to a kind of recycling of discarded polishing powder from rare earth Method.
Background technology：
Mostly important process is polishing process in material surface processing technology, and polishing powder is then in polishing processing One of critical material, be affected to the quality for being polished product.Polishing powder from rare earth is as important optical glass polishing material Material, has many advantages, such as, such as：Good, the higher density and hardness of good crystalline form, chemism, polishing efficiency are high, layer luminosity is steady Characteristics such as fixed and service life length, and be " king of polishing powder " by person, and gradually instead of it is other polish powder materials and It is rapidly progressed in polishing industry, is widely used in the essence of optical photoconductor glass, ornaments, building materials, mold and precision instrument Mill.
With the fast development of optics and electronic information science technology, optical glass demand increases, has driven dilute year by year The development of native polishing powder industry.2005, the market demand of global polishing powder from rare earth was about 20,000 tons, the rare earth polishing in China For powder consumption figure at 1~1.1 ten thousand tons or so, the dosage of China's polishing powder from rare earth accounts for about the half of world's aggregate consumption, becomes the world Polishing powder from rare earth produces and uses big country.2011, China's polishing powder from rare earth dosage reached 20,000 tons, China's rare earth in 2017 The consumption figure of polishing powder is expected to reach 100,000 tons or more.China has as Rare Earth Production big country, the production of polishing powder from rare earth Its only thick advantage, has driven developing for polishing industry, however as the increase of polishing powder from rare earth dosage, discards rare earth and throws Light powder yield also cumulative year after year, due in discarded polishing powder from rare earth not only containing polishing powder raw material, but also contain optics glass The ingredient of glass containing a large amount of lead element in optical glass, shows the toxicity of flint glass according to relevant result of study Greatly, although existing with glass volume morphing, once into water body or soil, water body and soil will be polluted, passed through Food chain enters human body, and finally the health of people is damaged.In view of the non-renewable and heavy metal of rare earth is for ring The pollution in border, if its recycling can have great importance for sustainable development and environmental protection.
Chinese patent (Publication No. CN104371555A) describes the condition for using nitric acid and hydrogen peroxide in heating The lower rare earth oxide by discarded polishing powder from rare earth dissolves, and the pH value of solution is adjusted with ammonium hydroxide, then in the item of heating Hydrogen peroxide and Ce (OH) are added under part4Suspension make rare-earth precipitation, through separation roast after obtain rare earth oxide.The patent A large amount of nitric acid can be consumed during rare earth element is leached, while lead can also dissolve out, cause the loss of lead, be unsuitable for being used for The extraction of heavy metal lead and rare earth element.Chinese patent (Publication No. CN101613802A) is described using vacuum carbon heat also Former method is destroyed the network structure of glass under high temperature and vacuum condition, is restored the lead in glass using carbon.It should Patent need the harsh reaction conditions such as higher temperature condition (temperature is 1000 DEG C) and vacuum (system pressure 10Pa) with Mating production equipment is difficult to realize industrialized production.Chinese patent (Publication No. CN102051487A) describes will be useless CRT glass dust, activated carbon and highly basic mixing are abandoned, after frit reaction, lead bullion, lye and alkaline residue is isolated, then uses dilute hydrochloric acid It embathes alkaline residue and extracts remaining lead, this patent is not to be restored lead by drastic reduction technology, and is also needed to using hydrochloric acid Alkaline residue is post-processed, this process consumes a large amount of hydrochloric acid.Rare earth, metallic lead and silicon are not suitable for it through analyzing the patent Separation.
Invention content：
It is an object of the present invention to provide a kind of recovery methods of discarded polishing powder from rare earth, and the method achieve the polishings of discarded rare earth The innoxious of powder, minimizing and recycling treatment meet the target that China develops a circular economy with energy-saving and emission-reduction.
To achieve the above object, the present invention uses following technical scheme：
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth, reducing agent and highly basic are taken, is uniformly mixed, obtains mixture；Wherein：It is described discarded dilute Contain ceria and glass dust in native polishing powder, contain lead oxide and silica in the glass dust；Additive amount is massaged That ratio, discards lead oxide in polishing powder from rare earth: solid carbon=(1: 1.24)~(1: 3.52) in reducing agent；Discarded polishing powder from rare earth Middle silica: highly basic=(1: 5.05)~(1: 9.47)；
(2) mixture is positioned in reaction vessel, carries out reduction reaction, obtain reduzate；Wherein：Reduction reaction temperature It is 600~800 DEG C to spend, and the reduction reaction time is 60~240min；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and aqueous silicate solution Lead；
(5) mixture of aqueous silicate solution and rich rare earth material obtains aqueous silicate solution and rich rare earth material by filtering.
In the step (1), polishing powder from rare earth granularity is discarded below 20 μm.
In the step (1), reducing agent granularity is below 120 mesh.
In the step (1), reducing agent is one kind in active powdered carbon, coke blacking or coal dust.
In the step (1), highly basic is sodium hydroxide or potassium hydroxide.
In the step (1), aqueous silicate solution is sodium silicate aqueous solution or potassium silicate aqueous solution.
In the step (1), hybrid manipulation carries out in batch mixer.
In the step (2), mixture is positioned in magnesia crucible, and magnesia crucible is positioned over reaction vessel In, carry out reduction reaction.
In the step (2), reaction vessel is heating furnace.
In the step (2), heating furnace is Muffle furnace.
In reduction process, the key reaction being related to is as follows：
PbO+C=Pb+CO
2PbO+C=2Pb+CO2
PbO+CO=Pb+CO2
SiO2+ 2NaOH=Na2SiO3+H2O
SiO2+ 2KOH=K2SiO3+H2O
Can efficiently separate discarded polishing powder from rare earth middle rare earth, lead and element silicon using the art of this patent.
The basic principle of method main process provided by the invention is as follows：
Lead element is present in glass dust in the form of Network modifier in discarded polishing powder from rare earth, and rare earth is with oxide shape Formula is individually present.And this patent destroys the network structure of vitreum by adding in highly basic, by highly basic and silicon dioxde reaction The silicate phase of low melting point is generated, lead oxide is released from stable glass phase network structure, to reach strengthened glass The purpose of lead element low temperature drastic reduction in powder, and the volatilization row using low-temperature reduction technical controlling lead element in reduction process For while destroying glass phase network structure by highly basic, good heat is provided to strengthen lead element low temperature drastic reduction technology Mechanical condition；On the other hand, the low melting point silicate phase that highly basic is formed with silicon dioxde reaction is not only created in reduction process A fused solution environment has been made, has also provided a good dynamics condition for the aggregation growth of metallic lead, simultaneously because molten Melt the presence of state silicate phase system, can not only oxygen be prevented inwardly to spread, but also can also effectively inhibit the volatilization of metallic lead, and then Improve the recovery rate of metallic lead；Active powdered carbon, coke blacking and coal dust are well known reducing agents, are mainly used for drastic reduction and discard Lead element forms metallic lead in polishing powder from rare earth；Rotary filter press technology is mainly the difference of specific gravity by substance, in rotary filter press Generated centrifugal force is of different sizes in the process, and then realizes the effective of discarded polishing powder from rare earth middle rare earth, lead and element silicon Separation is finally reached the comprehensive utilization purpose of discarded polishing powder from rare earth.
Beneficial effects of the present invention：
(1) present invention can effectively recycle ceria and flint glass powder (lead and silicon member in discarded polishing powder from rare earth Element), pollution of the heavy metal lead element to environment in discarded polishing powder from rare earth can be not only solved, but also also achieve discarded rare earth The recycling of valuable constituent element in polishing powder；
(2) pass through the raw material proportioning of the present invention and the setting of reduction reaction time so that reduction reaction is more thorough, energy By lead oxide Restore All into metallic lead.
(3) after processed by the invention, the rate of recovery of lead is up to more than 99.9%, in rich rare earth material and aqueous silicate solution Lead total amount is less than 0.05%, and the obtained concentrated crystallization treatment of aqueous silicate solution can be used as the raw material of industry.So as to fulfill Leaded the innoxious of discarded polishing powder from rare earth, minimizing and recycling treatment purpose, meet China and develop a circular economy and save The target of energy emission reduction.
Description of the drawings：
The recovery method process flow chart of the discarded polishing powder from rare earth of Fig. 1 present invention.
Specific embodiment：
With reference to embodiment, the present invention is described in further detail.
The purpose of the present invention is to provide a kind of new technology by leaded discarded polishing powder from rare earth recycling, below With reference to attached drawing, the preferred embodiments of the present invention will be described in detail, so that advantages and features of the invention can be easier to by ability Field technique personnel understanding, so as to make a clearer definition of the protection scope of the present invention.
In the embodiment of the present invention 1~5：
Discarded polishing powder from rare earth is crushed, ground and dried, granularity is below 20 μm；
The chemical composition of discarded polishing powder from rare earth, as shown in table 1；
Active powdered carbon, coke blacking or coal powder size are below 120 mesh.
Table 1
Embodiment 1
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth 10.013g, coke blacking (fixed carbon content is 89%) 0.194g and sodium hydroxide are weighed 17.842g is uniformly mixed in batch mixer, obtains mixture；Wherein：In molar ratio, lead oxide in polishing powder from rare earth is discarded: also Solid carbon=1 in former agent: 2.06；In molar ratio, silica in polishing powder from rare earth: sodium hydroxide=1: 5.05 is discarded；
(2) mixture is positioned in magnesia crucible, magnesia crucible is positioned in Muffle furnace, restore anti- Should, reduction reaction temperature is 800 DEG C, and the reduction reaction time is 120min, obtains reduzate；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and sodium silicate aqueous solution Lead；The surface of metallic lead is rinsed with clear water, the quality that metallic lead is weighed after drying is 1.433g, and the rate of recovery of metallic lead is 98.8%；
(5) mixture of sodium silicate aqueous solution and rich rare earth material obtains sodium silicate aqueous solution and rich rare earth material by filtering, CeO in rich rare earth material2Content for 12.2%, the content of lead is less than 0.05%.
Embodiment 2
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth 10.012g, active powdered carbon (fixed carbon content is 99%) 0.104g and hydroxide are weighed Sodium 17.840g is uniformly mixed in batch mixer, obtains mixture；Wherein：In molar ratio, lead oxide in polishing powder from rare earth is discarded: Solid carbon=1 in reducing agent: 1.24；In molar ratio, silica in polishing powder from rare earth: sodium hydroxide=1: 5.05 is discarded；
(2) mixture is positioned in magnesia crucible, magnesia crucible is positioned in Muffle furnace, restore anti- Should, reduction reaction temperature is 650 DEG C, and the reduction reaction time is 120min, obtains reduzate；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and sodium silicate aqueous solution Lead；The surface of metallic lead is rinsed with clear water, the quality that metallic lead is weighed after drying is 1.431g, and the rate of recovery of metallic lead is 98.7%；
(5) mixture of sodium silicate aqueous solution and rich rare earth material obtains sodium silicate aqueous solution and rich rare earth material by filtering, CeO in rich rare earth material2Content for 16.51%, the content of lead is less than 0.05%.
Embodiment 3
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth 10.011g, coal dust (fixed carbon content is 71%) 0.152g and sodium hydroxide are weighed 24.273g is uniformly mixed in batch mixer, obtains mixture；Wherein：In molar ratio, lead oxide in polishing powder from rare earth is discarded: also Solid carbon=1 in former agent: 1.29；In molar ratio, silica in polishing powder from rare earth: sodium hydroxide=1: 6.87 is discarded；
(2) mixture is positioned in magnesia crucible, magnesia crucible is positioned in Muffle furnace, restore anti- Should, reduction reaction temperature is 800 DEG C, and the reduction reaction time is 120min, obtains reduzate；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and sodium silicate aqueous solution Lead；The surface of metallic lead is rinsed with clear water, the quality that metallic lead is weighed after drying is 1.427g, and the rate of recovery of metallic lead is 98.4%；
(5) mixture of sodium silicate aqueous solution and rich rare earth material obtains sodium silicate aqueous solution and rich rare earth material by filtering, CeO in rich rare earth material2Content for 17.5%, the content of lead is less than 0.05%.
Embodiment 4
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth 10.006g, active powdered carbon (fixed carbon content is 99%) 0.296g and hydroxide are weighed Sodium 33.41g is uniformly mixed in batch mixer, obtains mixture；Wherein：In molar ratio, lead oxide in polishing powder from rare earth is discarded: Solid carbon=1 in reducing agent: 3.52；In molar ratio, silica in polishing powder from rare earth: sodium hydroxide=1: 9.47 is discarded；
(2) mixture is positioned in magnesia crucible, magnesia crucible is positioned in Muffle furnace, restore anti- Should, reduction reaction temperature is 600 DEG C, and the reduction reaction time is 240min, obtains reduzate；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and sodium silicate aqueous solution Lead；The surface of metallic lead is rinsed with clear water, the quality that metallic lead is weighed after drying is 1.432g, and the rate of recovery of metallic lead is 98.8%；
(5) mixture of sodium silicate aqueous solution and rich rare earth material obtains sodium silicate aqueous solution and rich rare earth material by filtering, CeO in rich rare earth material2Content for 16.63%, the content of lead is less than 0.05%.
Embodiment 5
A kind of recovery method of discarded polishing powder from rare earth, includes the following steps：
(1) discarded polishing powder from rare earth 10.021g, active powdered carbon (fixed carbon content is 99%) 0.184g and hydroxide are weighed Potassium 40.791g is uniformly mixed in batch mixer, obtains mixture；Wherein：In molar ratio, lead oxide in polishing powder from rare earth is discarded: Solid carbon=1 in reducing agent: 2.19；In molar ratio, silica in polishing powder from rare earth: potassium hydroxide=1: 8.24 is discarded；
(2) mixture is positioned in magnesia crucible, magnesia crucible is positioned in Muffle furnace, restore anti- Should, reduction reaction temperature is 750 DEG C, and the reduction reaction time is 60min, obtains reduzate；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metal of rich rare earth material and potassium silicate aqueous solution Lead；The surface of metallic lead is rinsed with clear water, the quality that metallic lead is weighed after drying is 1.431g, and the rate of recovery of metallic lead is 98.6%；
(5) mixture of potassium silicate aqueous solution and rich rare earth material obtains potassium silicate aqueous solution and rich rare earth material by filtering, CeO in rich rare earth material2Content for 16.6%, the content of lead is less than 0.05%.

Claims (8)

1. a kind of recovery method of discarded polishing powder from rare earth, which is characterized in that include the following steps：
(1) discarded polishing powder from rare earth, reducing agent and highly basic are weighed, is uniformly mixed, obtains mixture；Wherein：The discarded rare earth Contain ceria and glass dust in polishing powder, contain lead oxide and silica in the glass dust；Additive amount in molar ratio, Lead oxide in discarded polishing powder from rare earth: solid carbon=(1: 1.24)~(1: 3.52) in reducing agent；Two in discarded polishing powder from rare earth Silica: highly basic=(1: 5.05)~(1: 9.47)；
(2) mixture is positioned in reaction vessel, carries out reduction reaction, obtain reduzate；Wherein：Reduction reaction temperature is 600~800 DEG C, the reduction reaction time is 60~240min；
(3) by reduzate water quenching to room temperature, cooled product is obtained；
(4) cooled product is subjected to rotary filter press, obtains the mixture and metallic lead of rich rare earth material and aqueous silicate solution；
(5) mixture of aqueous silicate solution and rich rare earth material obtains aqueous silicate solution and rich rare earth material by filtering.
2. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (1), Discarded polishing powder from rare earth granularity is below 20 μm.
3. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (1), Reducing agent granularity is below 120 mesh.
4. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (1), Reducing agent is one kind in active powdered carbon, coke blacking or coal dust.
5. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (1), Highly basic is sodium hydroxide or potassium hydroxide.
6. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (1), Hybrid manipulation carries out in batch mixer.
7. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (2), Mixture is positioned in magnesia crucible, and magnesia crucible is positioned in reaction vessel, carries out reduction reaction.
8. the recovery method of discarded polishing powder from rare earth according to claim 1, which is characterized in that in the step (2), Reaction vessel is heating furnace.
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CN108037113B (en) * 2017-11-27 2020-09-25 西北矿冶研究院 Method for reducing and dissolving lanthanum-cerium-rare earth polishing powder by adopting liquid-solid phase

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CN102115822A (en) * 2010-11-18 2011-07-06 吴泉锦 Method for recovering rare earth oxide from fluorescent powder and polishing powder waste
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
WO2013128536A1 (en) * 2012-02-27 2013-09-06 株式会社アサカ理研 Method for separating rare earth elements from optical glass waste
CN104532006A (en) * 2015-01-26 2015-04-22 山东科技大学 Method for extracting europium oxide and yttrium oxide from waste fluorescent powder

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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
WO2013128536A1 (en) * 2012-02-27 2013-09-06 株式会社アサカ理研 Method for separating rare earth elements from optical glass waste
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
CN104532006A (en) * 2015-01-26 2015-04-22 山东科技大学 Method for extracting europium oxide and yttrium oxide from waste fluorescent powder

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