CN109022796A - A kind of low-temperature environment-friendly method from polished waste material recovering rare earth - Google Patents
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth Download PDFInfo
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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
- 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
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- 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
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Abstract
The invention discloses a kind of low-temperature environment-friendly methods from polished waste material recovering rare earth.Described method includes following steps: first polished waste material is ground up, sieved and be dipped into dilute hydrochloric acid obtain acidification polishing powder；Reducing agent and catalyst are added in hydrochloric acid and obtain mixing hydrochloric acid；Acidification polishing powder is added in mixing hydrochloric acid again and is dissolved, filtrate is obtained by filtration；Oxalic acid is added in filtrate to be precipitated, filters, dry, roast, ceria and lanthana can be obtained.The method of the invention can dissolve Ce by the collective effect of reducing agent, catalyst and diluted acid under conditions of low temperature, normal pressure, diluted acid4+, using low temperature and it is low in cost, easy to operate, the rare earth in polished waste material is recycled to equipment requirement and small, highly-safe, the environment amenable mode of loss；Also have the advantages that rare earth dissolution rate is high, rare earth yield is high simultaneously, has recycled the rare earth element in polished waste material, protected environment while creating value, there is important social and economic benefit.
Description
Technical field
The invention belongs to solid wastes recyclings to utilize technical field, make from optics, electronics industry more particularly, to one kind
The low-temperature environment-friendly method of recovering rare earth in discarded polishing powder after.
Background technique
Cerium-based rare earth polishing powder is important one of rare-earth products, has cutting power strong, and polishing time is short, polishes precision
The advantages that height, clean operation environment, referred to as " king of polishing powder ", it is widely used in plate glass, cathode-ray tube, TV
The polishing of the devices such as computer monitor, glass bulb, spectacle lens, optical glass, camera lens, jewel, crystal, ornament, China are annual
Polishing powder from rare earth usage amount is at 25000 tons/year, especially with China's mobile phone, the rapid development of liquid crystal display industry, rare earth
Polishing powder demand is being increased with the speed in year 15%.
Polished waste material is mainly by the solid slag of polishing powder from rare earth polishing waste liquid precipitation and separation, wherein mainly containing titanium dioxide
Cerium, there are also the mill skins (organic polymer) and waste liquid on part rare earth oxide containing lanthanum, the glass particle to be got off by mill, polishing machine
In artificial mixed precipitating reagent aluminium chloride etc., it is most of use after discarded polishing powder from rare earth be landfilled as solid waste,
On the one hand environmental pollution is caused, on the other hand rare earth resources is caused to be wasted.A large amount of year by year with China's rare earth resources develop,
It is necessary to recycle rare earth waste.
There are many methods of the recovering rare earth from polished waste material at present, mainly use acid-soluble method, and such as sulfuric acid process uses
98% concentrated sulfuric acid reaches 92.3% in 160 DEG C of heating 3h, the leaching rate of rare earth；Hydrochloric acid method, using 35.5% concentrated hydrochloric acid 95
DEG C heating 2h, it can be achieved that rare earth dissolve, thus by it is subsequent filtering, precipitating and roasting recycling obtain ceria；Nitric acid mistake
Hydrogen oxide method, using 50~72% nitric acid, the hydrogen peroxide that addition accounts for polishing powder quality 30~50% is molten in 60~80 DEG C of stirrings
Solve ceria recovering rare earth.But above by acid-soluble method from the method for polished waste material recovering rare earth high concentrated acid,
It is carried out under high temperature, working condition is harsh, corrodes equipment, and environmental pollution is big, while process costs are also high.Also have in room temperature or low temperature
The lower recovery process for promoting salt Ore Leaching using addition iron ammonium sulfate, iron filings, but the technique can generate a large amount of iron content containing ammonia
Waste water, environmental pollution are larger.
Therefore, it is badly in need of developing a kind of low-temperature environment-friendly method of recovering rare earth from polished waste material, makes rare earth element therein
It is reused, there is important social and economic benefit.
Summary of the invention
It is an object of the invention to need to carry out under high concentrated acid and high temperature for recovering rare earth method in the prior art,
Working condition is harsh, corrosion equipment, and environmental pollution is big, while process costs also high disadvantage and deficiency, provides a kind of from polishing
The low-temperature environment-friendly method of waste recovery rare earth.The method of the invention, can by the collective effect of reducing agent, catalyst and diluted acid
To dissolve insoluble Ce well under conditions of low temperature, normal pressure, diluted acid4+, using low temperature and it is low in cost, easy to operate,
Rare earth in polished waste material is recycled to equipment requirement and small, highly-safe, the environment amenable mode of loss；Also have simultaneously dilute
The advantage that native dissolution rate is high, rare earth yield is high, so that the rare earth element in polished waste material is recycled, while creating value
Environment is protected, there is important social and economic benefit.
Above-mentioned purpose of the invention is achieved by following scheme:
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, includes the following steps:
S1. polished waste material is ground and is sieved, remove the thick slag of bulky grain；
S2. polished waste material powder is dipped into the dilute hydrochloric acid of 0.01~2.0mol/L, acidification polishing powder is obtained after filtering；
S3. reducing agent and catalyst are added in the hydrochloric acid that concentration is 0.5~4mol/L, obtain mixing hydrochloric acid；
S4. acidification polishing powder according to mass concentration is that 0.01~60g/L is added in mixing hydrochloric acid, and it is heated to 35~
60 DEG C of dissolutions, are obtained by filtration filtrate；
S5. oxalic acid is added in filtrate and generates precipitating, precipitating is obtained by filtration and dries, roast, titanium dioxide can be obtained
Cerium and lanthana；
Reducing agent in step S3 be activated carbon, sludge carbon, carbon fiber, petroleum coke powder, carbon nanotube, expanded graphite or
Graphene；The mass concentration for mixing reducing agent in hydrochloric acid is 0.01~100g/L；
Catalyst in step S3 is fluorite, ice crystal or NaF；Mix hydrochloric acid in catalyst mass concentration be 0.01~
5g/L。
Cerium in polished waste material is with insoluble Ce4+In the presence of Ce hard to tolerate4+Usually only in high concentrated acid and high temperature item
It is just dissolved under part, and the present invention passes through the collective effect of reducing agent, catalyst and diluted acid, so that insoluble Ce4+In low temperature (phase
For using hot conditions in the prior art), normal pressure, can dissolve well in the presence of diluted acid, avoid using highly concentrated
It spends acid and hot conditions and leads to higher cost, the high requirements on the equipment, equipment loss is big, the serious problem of environmental pollution.
Reducing agent of the present invention is the solid kind reducing agent for being not dissolved in acid, economic and environment-friendly；To after reaction,
Reducing agent is easily separated out, renewable and reuse, and will not generate the waste water of pollution environment；Simultaneously because of the invention
The method is using diluted acid, and the waste liquid after reaction is easy recycling, and cost recovery is low, environmentally friendly；In addition this is used
When class reducing agent, the impurity in the rare earth material of recycling is less, will not introduce other impurity.
Since the rare earth oxide in polished waste material is difficult to be dissolved in dilute hydrochloric acid, in order to improve the rate of recovery of rare earth,
During rare earth dissolves, need to control the dosage and temperature of acidification polishing powder, reducing agent and catalyst, i.e. in step S4
Condition and parameter；If the too high levels or reducing agent of acidification polishing powder and the dosage of catalyst are too low, it is easy to cause rare earth
Dissolution rate decline, then the rate of recovery of rare earth also just reduces；And although temperature is higher, is more conducive to the dissolution of rare earth, it is same
When, temperature is excessively high and causes operating condition severe and hydrochloric acid is easy to cause to volatilize, and finally also results in the dissolution rate of rare earth and molten
Solve the decline of speed.Therefore, in order to improve rare earth yield and recycling rare earth material purity and rare earth recovery rate
And environmental issue, it is 35~60 DEG C by the dissolution conditions set temperature for being acidified polishing powder；It is acidified polishing powder, reducing agent and catalyst
Mass concentration be respectively 0.01~60g/L, 0.01~100g/L and 0.01~5g/L.
Preferably, 40~400 meshes are crossed after polished waste material grinding in step S1.
Preferably, the reducing agent using it is preceding at 20~60 DEG C at a temperature of first pass through mass percent be 1.0~
30.0% H2O2Or dosage is the O of 0.001~300.0mg/min3It carries out low-level oxidation and handles 0.1~10h.With it is untreated
Reducing agent compare, after low-level oxidation is handled, there are more reproducibility hydroxyls, i.e. reduction activation site in the surface of reducing agent more
It is more, be conducive to the reaction efficiency and reactivity that improve reducing agent.But if low-level oxidation extent control is bad, if hyperoxidation,
Be easy to cause active site further to be aoxidized, so as to cause reduction activation site inactivation, the reaction efficiency of reducing agent and
Reactivity reduces.
Preferably, the H2O2Mass percent be 2.0~10.0%；The O3Dosage be 0.2~10.0mg/
min；The temperature of the low-level oxidation processing is 25~40 DEG C.
Preferably, the H2O2Mass percent be 8.0%, low-level oxidation handle the time be 3h；The O3Dosage be
0.8mg/min, low-level oxidation handle the time as 0.5h；The temperature of the low-level oxidation processing is 25 DEG C.
Preferably, the reducing agent is activated carbon powder, sludge carbon, carbon fiber or petroleum coke powder.
Preferably, mass concentration of the reducing agent in mixing hydrochloric acid is 1~30g/L；The catalyst is in salt-mixture
Mass concentration in acid is 0.05~2g/L.
Preferably, the concentration of hydrochloric acid is 0.5~2.0mol/L in step S2 and S3；Polished waste material powder impregnates in step S2
Time is 1~72h.It is in order to remove some impurity for being dissolved in acid, to mention that polished waste material powder, which is now carried out acidification, in step S2
The purity for the rare earth that high subsequent recovery arrives.
Preferably, polished waste material powder soaking time is 1~10h in step S2.
Preferably, it is 1~30g/L that mass concentration of the polishing powder in mixing hydrochloric acid is acidified in step S4；Heating temperature is
45~55 DEG C.Under the conditions of this temperature, it not only can guarantee that the rate of dissolution of rare earth element will not be too low, but also can guarantee the volatilization of hydrochloric acid
Amount reduces, and finally obtains the rate of dissolution and meltage of high rare earth element.
Preferably, the concentration of oxalic acid described in step S5 is 2mol/L；The temperature of the roasting is 400~1100 DEG C.
The temperature of roasting is higher, and the decomposition efficiency of oxalic acid is higher, and obtain cerium oxide crystallization degree and particle it is bigger, temperature
It is smaller to spend lower obtained cerium oxide particle, opitimum temperature can be determined depending on the purposes of recovering rare earth, and when roasting temperature
When degree is more than 1100 DEG C, scratch can be left when the polishing material of recycling is used as polishing powder on glass instead, influence glass
Presentation quality.
Compared with prior art, the invention has the following advantages:
The method of the invention, can be in low temperature, normal pressure, diluted acid by the collective effect of reducing agent, catalyst and diluted acid
Under conditions of dissolve insoluble Ce well4+, using low temperature and it is low in cost, easy to operate, to equipment requirement and loss it is small,
Highly-safe, environment amenable mode recycles the rare earth in polished waste material；Also there is rare earth dissolution rate height, rare earth recovery simultaneously
The high advantage of rate protects environment while creating value so that the rare earth element in polished waste material is recycled, and has important
Social and economic benefit.
Detailed description of the invention
Fig. 1 is rare earth dissolution rate and rate of recovery result in Examples 1 to 4.
Specific embodiment
The present invention is made combined with specific embodiments below and further being elaborated, the embodiment is served only for explaining this
Invention, is not intended to limit the scope of the present invention.Test method as used in the following examples is normal unless otherwise specified
Rule method；Used material, reagent etc., unless otherwise specified, for the reagent and material commercially obtained.
Embodiment 1
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 1.0mol/L, stirring 5h processing is filtered
To acidification polishing powder solid after purification；
(3) 1.5g activated carbon is added to 50mL 1.37mol/L salt as reducing agent, 0.025g fluorite as catalyst
In acid, the mixing hydrochloric acid solution containing reducing agent and catalyst is obtained；
(4) acidification polishing powder solid is added in mixing hydrochloric acid solution, consolidates polishing powder in 55 DEG C of at a temperature of stirring
After body dissolves 1h, activated carbon and undissolved SiO are filtered to isolate2Equal impurity, obtain containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filtering, drying, 400
After DEG C roasting, recycling obtains 0.61g rare earth oxide, it is contemplated that content in polishing powder containing rare earth is 73%, by conversion, is obtained
The rate of recovery to rare earth is 83.6%.
Wherein, reducing agent activated carbon advanced low-level oxidation can also be handled according to the following steps using preceding: by 1.5g activity
Carbon is added in 8% hydrogen peroxide after 25 DEG C of processing 3h, and the activated carbon of surface low-level oxidation processing is obtained after filtration washing；With this
For the processed active carbon of low-level oxidation instead of untreated activated carbon in above-mentioned steps (3) as reducing agent, other conditions are constant, return
Receipts obtain 0.65g rare earth oxide, i.e. the rate of recovery of rare earth is 89.0%.
Embodiment 2
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 2.0mol/L, stirring 2h processing is filtered
To acidification polishing powder solid after purification；
(3) 2.0g sludge carbon is added to 50mL 2.5mol/L salt as reducing agent, 0.01g ice crystal as catalyst
In acid, the mixing hydrochloric acid solution containing reducing agent and catalyst is obtained；
(4) acidification polishing powder solid is added in mixing hydrochloric acid solution, consolidates polishing powder in 35 DEG C of at a temperature of stirring
After body dissolves 6h, sludge carbon and undissolved SiO are filtered to isolate2Equal impurity, obtain containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filtering, drying, 600
After DEG C roasting, recycling obtains 0.58g rare earth oxide, it is contemplated that content in polishing powder containing rare earth is 73%, by conversion, is obtained
The rate of recovery to rare earth is 79.4%.
Wherein, reducing agent activated carbon advanced low-level oxidation can also be handled according to the following steps using preceding: by 2.0g sludge
Carbon is added to the ozone of 0.8mg/min ozone dosage after 25 DEG C of processing 0.5h, is obtained at the low-level oxidation of surface after filtration washing
The sludge carbon of reason replaces above-mentioned untreated sludge carbon as reducing agent using the sludge carbon of this low-level oxidation processing, and other conditions are not
Become, recycling obtains 0.62g rare earth oxide, i.e. the rate of recovery of rare earth is 84.9%.
Embodiment 3
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 0.5mol/L, stirring 10h processing is filtered
To acidification polishing powder solid after purification；
(3) 1.0g carbon fiber is added to 50mL 1.37mol/L salt as reducing agent, 0.025g fluorite as catalyst
In acid, the mixing hydrochloric acid solution containing reducing agent and catalyst is obtained；
(4) acidification polishing powder solid is added in mixing hydrochloric acid solution, consolidates polishing powder in 45 DEG C of at a temperature of stirring
After body dissolves 3h, activated carbon and undissolved SiO are filtered to isolate2Equal impurity, obtain containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filtering, drying, 800
After DEG C roasting, recycling obtains 0.50g rare earth oxide, it is contemplated that content in polishing powder containing rare earth is 73%, by conversion, is obtained
The rate of recovery to rare earth is 68.5%.
Wherein, reducing agent activated carbon advanced low-level oxidation can also be handled according to the following steps using preceding: by 1.0g carbon fiber
Dimension is added to the ozone of 0.2mg/min ozone dosage after 25 DEG C of processing 0.5h, is obtained at the low-level oxidation of surface after filtration washing
The carbon fiber of reason replaces above-mentioned untreated carbon fiber as reducing agent using the carbon fiber of this low-level oxidation processing, and other conditions are not
Become, recycling obtains 0.55g rare earth oxide, i.e. rare earth yield is 75.3%.
Embodiment 4
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 0.5mol/L, stirring 10h processing is filtered
To acidification polishing powder solid after purification；
(3) 3.0g petroleum coke powder is added to 50mL 2.5mol/ as reducing agent, 0.01g ice crystal as catalyst
In L hydrochloric acid, the mixing hydrochloric acid solution containing reducing agent and catalyst is obtained；
(4) acidification polishing powder solid is added in mixing hydrochloric acid solution, consolidates polishing powder in 55 DEG C of at a temperature of stirring
After body dissolves 1h, activated carbon and undissolved SiO are filtered to isolate2Equal impurity, obtain containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filter, dry,
After 1100 DEG C of roastings, recycling obtains 0.45g rare earth oxide, it is contemplated that the content in polishing powder containing rare earth is 73%, by changing
It calculates, the rate of recovery for obtaining rare earth is 61.6%.
Wherein, reducing agent activated carbon advanced low-level oxidation can also be handled according to the following steps using preceding: by 1.0g carbon fiber
Dimension is added to the ozone of 0.2mg/min ozone dosage after 25 DEG C of processing 0.5h, is obtained at the low-level oxidation of surface after filtration washing
The petroleum coke powder of reason replaces above-mentioned untreated petroleum coke powder as reduction using the petroleum coke powder of this low-level oxidation processing
Agent, other conditions are constant, and recycling obtains 0.51g rare earth oxide, the rate of recovery 69.9%.
Comparative example 1
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 1.0mol/L, stirring 5h processing is filtered
To acidification polishing powder solid after purification；
(3) polishing powder after above-mentioned acidification is added in the hydrochloric acid of 5.7mL 6mol/L, while iron powder 0.07g is added,
It is heated to boiling, divides 10 times and add iron powder 0.14g, each 0.014g；
(4) it filters, isolates SiO2Equal impurity, obtain containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filter, dry,
After 1050 DEG C of roastings, recycling obtains the mixture of 0.58g rare earth oxide and iron oxide, wherein the percentage of rare earth and iron oxide
Respectively 70.7% and 29.3%, i.e., the 0.17g containing iron oxide of 0.41g containing rare earth oxide in mixture, it is contemplated that in polishing powder
Content containing rare earth is 73%, and by conversion, the rate of recovery for obtaining rare earth is 56.2%.
When changing reducing agent into iron, the rate of recovery of rare earth is not only decreased obviously, but also containing a large amount of in the rare earth recycled
Iron oxides impurities, influence recycling rare earth material subsequent applications.
Comparative example 2
A kind of low-temperature environment-friendly method from polished waste material recovering rare earth, detailed process is as follows:
(1) after grinding polished waste material, short grained throwing is obtained to remove the thick slag of bulky grain with the sieve of 40 mesh
Waste photopolymer；
(2) 1.0g little particle polished waste material is added in the dilute hydrochloric acid of 50mL 0.5mol/L, stirring 10h processing is filtered
To acidification polishing powder solid after purification；
(3) it is added in 50mL 2.5mol/L hydrochloric acid, obtains mixed containing catalyst using 0.01g ice crystal as catalyst
Close hydrochloric acid solution；
(4) acidification polishing powder solid is added in mixing hydrochloric acid solution, consolidates polishing powder in 55 DEG C of at a temperature of stirring
After body dissolves 1h, undissolved SiO is filtered to isolate2Deng obtaining containing Ce3+Filtrate；
(5) agent of 2.0mol/L oxalic acid precipitation is added into filtrate to generate until precipitating without new discoloration, filtering, drying, 800
After DEG C roasting, recycling obtains 0.05g rare earth oxide, it is contemplated that content in polishing powder containing rare earth is 73%, by conversion, is obtained
The rate of recovery to rare earth is 6.8%.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of shield range can also be made on the basis of above description and thinking for those of ordinary skill in the art
Other various forms of variations or variation, there is no necessity and possibility to exhaust all the enbodiments.It is all of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (10)
1. a kind of low-temperature environment-friendly method from polished waste material recovering rare earth, which comprises the steps of:
S1. polished waste material is ground and is sieved, remove the thick slag of bulky grain；
S2. polished waste material powder is dipped into the dilute hydrochloric acid of 0.01~2.0mol/L, acidification polishing powder is obtained after filtering；
S3. reducing agent and catalyst are added in the hydrochloric acid that concentration is 0.5~4mol/L, obtain mixing hydrochloric acid；
It S4. is that 0.01~60g/L is added in mixing hydrochloric acid, and is heated to 35~60 according to mass concentration by acidification polishing powder
DEG C dissolution, filtrate is obtained by filtration；
S5. by oxalic acid be added in filtrate generate precipitating, precipitating is obtained by filtration and dries, roast, can be obtained ceria and
Lanthana；
Reducing agent in step S3 is activated carbon, sludge carbon, carbon fiber, petroleum coke powder, carbon nanotube, expanded graphite or graphite
Alkene；The mass concentration for mixing reducing agent in hydrochloric acid is 0.01~100 g/L；
Catalyst in step S3 is fluorite, ice crystal or NaF；The mass concentration for mixing catalyst in hydrochloric acid is 0.01~5 g/
L。
2. according to claim 1 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that the reducing agent
The H for being 1.0~30.0% by mass percent at a temperature of using preceding elder generation at 20~60 DEG C2O2Or dosage be 0.001~
300.0 the O of mg/min3It carries out low-level oxidation and handles 0.1~10h.
3. according to claim 2 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that the H2O2's
Mass percent is 2.0~10.0%；The O3Dosage be 0.2~10.0 mg/min；The temperature of the low-level oxidation processing
It is 25~40 DEG C.
4. according to claim 3 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that the H2O2's
Mass percent is 8.0%, and low-level oxidation handles the time as 3h；The O3Dosage be 0.8 mg/min, low-level oxidation handle the time
For 0.5h；The temperature of the low-level oxidation processing is 25 DEG C.
5. according to claim 1 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that the reducing agent
For activated carbon powder, sludge carbon, carbon fiber or petroleum coke powder.
6. according to claim 5 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that the reducing agent
Mass concentration in mixing hydrochloric acid is 1~30 g/L；Mass concentration of the catalyst in mixing hydrochloric acid is 0.05~2
g/L。
7. according to claim 1 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that step S2 and S3
The concentration of middle hydrochloric acid is 0.5~2.0mol/L；Polished waste material powder soaking time is 1~72h in step S2.
8. according to claim 7 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that thrown in step S2
Waste photopolymer powder soaking time is 1~10h.
9. according to claim 1 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that sour in step S4
Changing mass concentration of the polishing powder in mixing hydrochloric acid is 1~30g/L；Heating temperature is 45~55 DEG C.
10. according to claim 1 from the low-temperature environment-friendly method of polished waste material recovering rare earth, which is characterized in that in step S5
The concentration of the oxalic acid is 2mol/L；The temperature of the roasting is 400~1100 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| US11753308B1 (en) | 2020-12-02 | 2023-09-12 | Beijing University Of Technology | Method for separating and extracting rare-earth and regenerating rare-earth polishing powder from rare-earth polishing powder waste |
| CN111039495B (en) * | 2020-01-06 | 2024-05-17 | 湖南景翌湘台环保高新技术开发有限公司 | Comprehensive recovery method of waste rare earth polishing powder and steel pickling waste liquid |
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