CN114700180A - Method for recovering rare earth components in waste polishing powder - Google Patents
Method for recovering rare earth components in waste polishing powder Download PDFInfo
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- CN114700180A CN114700180A CN202210279767.7A CN202210279767A CN114700180A CN 114700180 A CN114700180 A CN 114700180A CN 202210279767 A CN202210279767 A CN 202210279767A CN 114700180 A CN114700180 A CN 114700180A
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
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- B03D2201/04—Frothers
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
According to the failure reason of the polishing powder, firstly, the rare earth oxide is exposed through crushing and crushing processes, other pollutants on the surface of the rare earth oxide are further removed through oxalic acid cleaning, the crystal face of the rare earth oxide is exposed, and then the rare earth oxide is collected through a high-efficiency collecting agent in the flotation process, so that the recovery of the rare earth component is realized. The invention selects the rare earth components in the waste polishing powder as concentrate through the working procedures of drying dehydration, crushing, ore grinding, cleaning, flotation, dehydration filtration, drying and the likeAnd the polishing powder can be recycled as polishing powder. Meanwhile, after the rare earth components are floated, most of the remaining tailings are SiO2And Al2O3With the mature technology development, the method can be used for the synthesis and manufacture of sodalite in future, and the production of tailings-free ores is realized.
Description
Technical Field
The invention belongs to the technical field of rare earth material recovery, and particularly relates to a method for recovering rare earth components in waste polishing powder.
Background
With the increasing requirements for the performance of polishing products, the research on polishing technology and polishing materials is being conducted deeply and improved. Particularly, the rare earth polishing powder grinding material used in the glass industry has the advantages of moderate hardness, strong cutting capability, short polishing time, high polishing precision, long service life, clean and environment-friendly operation environment and the like by virtue of the similar hardness and unique crystal structure of the rare earth oxide with the glass. Therefore, the rare earth polishing powder is widely used in the polishing industry. According to statistics, the yield of the rare earth polishing powder reaches 2.2 ten thousand tons in 2016, and the yield of the rare earth polishing powder is increased at a rate of 10-20% per year.
In the polishing powder grinding and polishing process, the polishing powder is subjected to combined action of physical grinding and chemical grinding, the polishing powder is gradually lost under the action, about 70 percent of the lost rare earth polishing powder is converted into waste rare earth polishing powder, and the waste rare earth polishing powder is enriched and accumulated to form industrial waste, wherein the main component of the waste rare earth polishing powder is a rare earth compound; organic substances such as a precipitant and a flocculant; waste slag generated by the polished workpiece; polishing pad throws, and the like.
With the rare earth resource as a mineral resource which is developed strategically in China, the economic value and the social position of the rare earth resource are obviously improved. China has limited rare earth resources and generates a large amount of waste rare earth polishing powder every year, so that the increasing of the recycling of rare earth polishing powder waste is urgent. At present, the recycling range of polishing powder in China is small, the method is limited to the research and development stage of a laboratory, and most methods are acid-base leaching combined roasting treatment. If the methods are applied to actual industrial production, a large amount of acid and alkali has huge potential safety hazards in production and use, and a large amount of waste gas and waste liquid can be generated to pollute the environment. Meanwhile, high-temperature roasting has high energy consumption and generates a large amount of harmful gas. The methods have high cost and great harm, and are not suitable for practical industrial recycling.
Disclosure of Invention
The invention aims to provide a method for recovering rare earth components in waste polishing powder, which has the advantages of simple process, low cost and high product grade.
The method for recovering the rare earth components in the waste polishing powder comprises the following steps:
1) collecting the polishing powder waste residues after polishing, and then drying at a set temperature to obtain dried polishing powder waste residues;
2) carrying out primary crushing on the polishing powder waste residue dried in the step 1), and further carrying out ore grinding and crushing in ore grinding equipment after crushing is finished to obtain ore ground waste residue;
3) putting the waste residue after ore grinding in the step 2) into an oxalic acid solution for cleaning, and filtering after cleaning to obtain the cleaned waste residue;
4) placing the waste residue cleaned in the step 3) into a flotation tank, adding a flotation reagent and adjusting a flotation process for flotation to obtain concentrate, namely the rare earth component.
In the step 1), the drying temperature is 80-90 ℃, and the drying time is 7-8 h.
In the step 2), the primary crushing is carried out until the granularity of the polishing powder waste residue is 0.5-1.5 cm; grinding until the granularity of the ground product is less than 0.038mm and is over 75 percent.
In the step 3), the solid-to-liquid ratio of the ground waste residue to the oxalic acid solution is 1 (1-3), and the mass concentration of the oxalic acid solution is 10-20%; the cleaning is stirring cleaning, and the cleaning time is 8-12 min.
In the step 4), a flotation process of one coarse, four fine and three sweeps is adopted for flotation; the flotation reagent comprises: pH regulator, inhibitor, collector and foaming agent; the pH regulator is sulfuric acid, the inhibitor is sodium fluosilicate, the collecting agent is a combined agent consisting of benzohydroxamic acid, sodium oleate, cocoamine and betaine in a mass ratio of (3-5) - (0.5-1.5) - (0.5), and the foaming agent is 2# oil; the concentration of the floated ore pulp is 20-40%; the rotation speed during the flotation is 1200-1600 r/min.
Preferably, the specific process of flotation comprises the following steps:
s1, adding a flotation reagent for roughing to obtain roughed concentrate and roughed tailings;
and S2, carrying out 3 times of scavenging on the roughed tailings in the step S1.
S3: and (5) carrying out four times of concentration on the rough concentrate obtained in the step S1 to obtain the concentrate containing the rare earth components.
In the step S1, the medicament system is roughly selected as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.8-2.2 kg/t, the addition amount of the collector relative to the raw ore is 1.8-2.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1-0.3 kg/t.
In the step S2, the first scavenging and the second scavenging require the addition of a chemical, and the third scavenging does not add a chemical; the medicament system for the first scavenging is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.0-1.4 kg/t, the addition amount of the collector relative to the raw ore is 1.2-1.6 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.08-0.12 kg/t; the second scavenging medicament system is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 0.8-1.2 kg/t, the addition amount of the collector relative to the raw ore is 1.0-1.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.05-0.08 kg/t.
In the step S3, the first to third concentration needs to be added with chemicals, the fourth concentration needs not to be added with chemicals, and the chemical system of the first concentration is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.4-1.8 kg/t, the addition amount of the collector relative to the raw ore is 1.6-2.0 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1-0.2 kg/t; the second selection is carried out according to the following medicament system: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.0-1.4 kg/t, the addition amount of the collector relative to the raw ore is 1.2-1.5 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.09-0.12 kg/t; the third selection medicament system is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 0.8-1.0 kg/t, the addition amount of the collector relative to the raw ore is 1.0-1.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.05-0.08 kg/t.
In the steps S2 and S3, the coarse middling products obtained in the scavenging process are returned to the upper-stage flotation to be used as feed; the fine middlings obtained in the concentration process are returned to the last stage of flotation as feed.
The tailings produced by the flotation process can be used as a raw material for preparing sodalite.
The principle of the invention is as follows: the invention focuses on exploring the optimal selection of agents and the mechanism of action of agents. According to the failure reason of the polishing powder, impurity particles generated in the polishing process can be gathered on the surface of the rare earth oxide, so that Si-OH is coated on CeO2Surface of the particles, and surface Ce3+Ce-O-Si is formed. Meanwhile, other additives are polluted in the polishing process, so that the original waste material after ore grinding is cleaned by oxalic acid, and the purpose is to clean pollutants coated on rare earth oxide to expose the crystal surfaces of cerium oxide and lanthanum oxide, so that a flotation reagent is better selected and collected; the benzohydroxamic acid, sodium oleate, cocoamine and betaine are combined to be used as a collecting combined medicament, and the effect of recovering rare earth from polishing powder waste residues is good. The benzohydroxamic acid forms a five-membered chelate ring with metal ions on the surface of a mineral through an O atom on a carbonyl group and an O atom on N, and generates characteristic adsorption on the surface of a rare earth oxide, so that the selectivity is better; the sodium oleate is used as a fatty acid collecting agent, has a longer carbon chain, is good in hydrophobicity, is beneficial to the foam flotation of rare earth, and has strong collecting capability on rare earth elements; the cocoamine and the betaine have excellent emulsification, dispersion and solubilization effects. In particular, betaine, as an amphoteric surfactant, has a rich foaming property in addition to the above-mentioned effects, and is useful as a foaming agent or a foam stabilizer. When the modified starch is compounded with an anionic surfactant, strong interaction is generated among molecules, and the foam increasing and viscosity increasing effects are obviously improved.
The invention has the beneficial effects that: according to the failure reason of the polishing powder, the rare earth oxide is exposed through the crushing and crushing process, other pollutants on the surface of the rare earth oxide are further removed through oxalic acid cleaning, the crystal face of the rare earth oxide is exposed, and then the efficient collecting agent is usedThe rare earth is collected in the flotation process, so that the recovery of the rare earth components is realized. According to the invention, through the working procedures of drying dehydration, crushing, ore grinding, cleaning, flotation, dehydration filtration, drying and the like, rare earth components in the waste polishing powder are selected as concentrate, and can be used as polishing powder for recycling. Meanwhile, after the rare earth components are floated, most of the remaining tailings are SiO2And Al2O3With the mature technology development, the method can be used for the synthesis and manufacture of sodalite in future, and the production of tailings-free ores is realized. The method completely recycles the waste polishing powder, greatly saves rare earth resources, reduces the recycling cost, has low harm to the environment in the whole production process, effectively solves the problem of processing the polishing powder waste in the industry at present, and realizes the ambitious goal of sustainable health development advocated by the state.
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FIG. 1A flow chart of a specific process in example 1.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available.
Example 1
The raw materials used in this example are from Changsha blue Cisco technology, Inc., and the production waste is obtained after polishing and grinding. Wherein the grade of cerium oxide is 46.64%, the grade of lanthanum oxide is 13.55%, and other main impurities are SiO2And Al2O3The grades are 15.67% and 11.99%, respectively. The process is shown as figure 1, and comprises the following steps:
the collected waste polishing powder is baked at 80 ℃ for 8 hours and completely dehydrated and then starts to be crushed. After the waste material is crushed to 0.5-1.5 cm by a crusher, the waste material is ground by a vibration grinding machine, and the condition is controlled so that the granularity of the ground product is less than 0.038mm and accounts for more than 75%. And then putting the ground waste residue into a stirrer, adding oxalic acid with the mass concentration of 15% according to the solid-liquid ratio of 1g to 2mL, and stirring and cleaning for 10 minutes at the rotating speed of 400-500 r/min. After the oxalic acid is cleaned and stirred, the oxalic acid is dewatered and filtered, and then the cleaned waste is put into a flotation machine to start flotation.
The flotation adopts a closed flotation process of coarse flotation, fine flotation and fine flotation, the feeding speed is controlled, the water adding amount is adjusted, the concentration of slurry is controlled at 30%, and the rotating speed is controlled at 1500r/min during flotation. Adding sulfuric acid solution to adjust pH to 3.0, sequentially adding sodium fluosilicate inhibitor (2 kg/t relative to the amount of raw ore) to inhibit SiO2And Al2O3(ii) a Adding a combination of benzohydroxamic acid, sodium oleate, cocoanut oil amine and betaine (the addition amount of the combination collector relative to the raw ore is 2kg/t) in a mass ratio of 4:4:1:1 of a combined collector, and collecting rare earth oxide (CeO)2、La2O3、CeOF2LaOF); then adding a foaming agent No. 2 for foaming (the addition amount of the foaming agent is 0.2kg/t relative to the raw ore), and starting roughing after aeration to obtain rough concentrate and rough tailings.
Scavenging the coarse tailings for 3 times, sequentially returning the scavenged coarse middlings to the previous stage of flotation to serve as feed, adding a medicament for each scavenging and the second scavenging, and adding no medicament for the third time; the medicament system for the first scavenging is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.0; the addition amount of the inhibitor relative to the raw ore is 1.2kg/t, the addition amount of the collector relative to the raw ore is 1.5kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1 kg/t; the second scavenging medicament system is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3; the addition amount of the inhibitor relative to the raw ore is 1.0kg/t, the addition amount of the collector relative to the raw ore is 1.2g/t, and the addition amount of the foaming agent relative to the raw ore is 0.08 kg/t.
Carrying out four-time concentration on the rough concentrates, wherein each selected concentrate is used as a feed for the next concentration, the concentrated middlings return to the previous stage of flotation, medicaments are required to be added for the first-time to third-time concentration, the medicaments are not required to be added for the fourth-time concentration, and the medicament system for the first concentration is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.0; the addition amount of the inhibitor relative to the raw ore is 1.6kg/t, the addition amount of the collector relative to the raw ore is 1.8kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.15 kg/t; the second selection is carried out according to the following medicament system: adding a pH regulator to regulate the pH value of the ore pulp to 3.0; the addition amount of the inhibitor relative to the raw ore is 1.2kg/t, the addition amount of the collector relative to the raw ore is 1.5kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1 kg/t; the third selection medicament system is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.0; the addition amount of the inhibitor relative to the raw ore is 1.0kg/t, the addition amount of the collector relative to the raw ore is 1.2kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.08 kg/t. Finally obtaining the rare earth component concentrate.
And (3) detecting the content of the rare earth components in the concentrate, wherein the total grade of cerium oxide and lanthanum oxide is 90%. Meanwhile, the recovery rate of the rare earth components is calculated to be higher than 70%, which shows that the method for recovering the waste polishing powder by adopting the flotation method is a feasible and effective means.
Example 2
The raw materials used in this example are from Changsha blue Cisco technology, Inc., and the production waste is obtained after polishing and grinding. Wherein the grade of cerium oxide is 42.35%, the grade of lanthanum oxide is 15.56%, and other main impurities are SiO2And Al2O3The grades are 17.54% and 13.87%, respectively.
The collected waste polishing powder is baked at 80 ℃ for 8 hours and completely dehydrated and then starts to be crushed. After the waste material is crushed to 0.5-1.5 cm by a crusher, the waste material is ground by a vibration grinding machine, and the condition is controlled so that the granularity of the ground product is less than 0.038mm and accounts for more than 75%. And then putting the ground waste residue into a stirrer, adding oxalic acid with the mass concentration of 15% according to the solid-liquid ratio of 1g to 3mL, and stirring and cleaning for 8 minutes at the rotating speed of 400-500 r/min. After the oxalic acid is cleaned and stirred, the oxalic acid is dewatered and filtered, and then the cleaned waste is put into a flotation machine to start flotation.
The flotation adopts closed-circuit flotation of one coarse, four fine and three sweepsThe flow controls the concentration of slurry to be 25% by controlling the feeding speed and adjusting the water adding amount, and the rotating speed is controlled to be 1600r/min during the flotation. Adding sulfuric acid solution to adjust pH to 3.5, sequentially adding sodium fluosilicate inhibitor (2.2 kg/t relative to the amount of raw ore) to inhibit SiO2And Al2O3(ii) a Adding a combination of benzohydroxamic acid, sodium oleate, cocoamine and betaine (the addition amount of the combination collector relative to raw ore is 2.2kg/t) in a combined collector mass ratio of 3:5:1.5:1.5, and collecting rare earth oxide (CeO)2、La2O3、CeOF2LaOF); then adding a foaming agent No. 2 for foaming (the addition amount of the foaming agent is 0.1kg/t relative to the raw ore), and starting roughing after aeration to obtain rough concentrate and rough tailings.
Scavenging the coarse tailings for 3 times, sequentially returning the scavenged coarse middlings to the previous stage of flotation to serve as feed, adding a medicament for each scavenging and the second scavenging, and adding no medicament for the third time; the medicament system for the first scavenging is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.5; the addition amount of the inhibitor relative to the raw ore is 1.0kg/t, the addition amount of the collector relative to the raw ore is 1.2kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.08 kg/t; the second scavenging medicament system is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.5; the addition amount of the inhibitor relative to the raw ore is 0.8kg/t, the addition amount of the collector relative to the raw ore is 1.0g/t, and the addition amount of the foaming agent relative to the raw ore is 0.06 kg/t.
Carrying out four-time concentration on the rough concentrates, wherein each selected concentrate is used as a feed for the next concentration, the concentrated middlings return to the previous stage of flotation, medicaments are required to be added for the first-time to third-time concentration, the medicaments are not required to be added for the fourth-time concentration, and the medicament system for the first concentration is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.5; the addition amount of the inhibitor relative to the raw ore is 1.4kg/t, the addition amount of the collector relative to the raw ore is 1.6kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1 kg/t; the second selection is carried out according to the following medicament system: adding a pH regulator to regulate the pH value of the ore pulp to 3.5; the addition amount of the inhibitor relative to the raw ore is 1.0kg/t, the addition amount of the collector relative to the raw ore is 1.2kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.09 kg/t; the medicament system selected for the third time is as follows: adding a pH regulator to regulate the pH value of the ore pulp to 3.5; the addition amount of the inhibitor relative to the raw ore is 0.8kg/t, the addition amount of the collector relative to the raw ore is 1.0kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.05 kg/t. Finally obtaining the rare earth component concentrate.
And (3) detecting the content of the rare earth components in the concentrate, wherein the total grade of cerium oxide and lanthanum oxide is 88.79%. Meanwhile, the recovery rate of the rare earth components is calculated to be higher than 72%, which shows that the method for recovering the waste polishing powder by adopting the flotation method is a feasible and effective means.
The above examples are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts thereof should be covered by the scope of the present invention.
Claims (10)
1. A method for recovering rare earth components in waste polishing powder comprises the following steps:
1) collecting the polishing powder waste residues after polishing, and then drying at a set temperature to obtain dried polishing powder waste residues;
2) carrying out primary crushing on the polishing powder waste residue dried in the step 1), and further crushing in ore grinding equipment after crushing is finished to obtain ore ground waste residue;
3) putting the waste residue after ore grinding in the step 2) into an oxalic acid solution for cleaning, and filtering after cleaning to obtain the cleaned waste residue;
4) placing the waste residue cleaned in the step 3) into a flotation tank, adding a flotation reagent and adjusting a flotation process for flotation to obtain concentrate, namely the rare earth component.
2. The method for recycling rare earth components from waste polishing powder according to claim 1, wherein in the step 1), the drying temperature is 80-90 ℃ and the drying time is 7-8 h.
3. The method for recycling rare earth components from waste polishing powder according to claim 1, wherein in the step 2), the waste polishing powder is primarily crushed until the granularity of the waste polishing powder is 0.5-1.5 cm; grinding ore until the granularity of the product is less than 0.038mm and is more than 75%.
4. The method for recycling rare earth components from waste polishing powder according to claim 1, wherein in the step 3), the solid-to-liquid ratio of the waste residue after ore grinding to the oxalic acid solution is 1 (1-3), and the mass concentration of the oxalic acid solution is 10-20%; the cleaning is stirring cleaning, and the cleaning time is 8-12 min.
5. The method for recycling rare earth components from waste polishing powder as claimed in claim 1, wherein in the step 4), flotation is performed by a one-coarse four-fine three-sweep flotation process; the flotation reagent comprises: pH regulator, inhibitor, collector and foaming agent; the pH regulator is sulfuric acid, the inhibitor is sodium fluosilicate, the collecting agent is a combined agent consisting of benzohydroxamic acid, sodium oleate, cocoamine and betaine in a mass ratio of (3-5) to (0.5-1.5), and the foaming agent is 2# oil; the concentration of the ore pulp subjected to flotation is 20-40%; the rotation speed during the flotation is 1200-1600 r/min.
6. The method for recovering rare earth components from waste polishing powder according to claim 5, wherein the flotation is carried out by the following specific process:
s1, adding a flotation reagent for roughing to obtain roughed concentrate and roughed tailings;
s2, carrying out 3 times of scavenging on the roughed tailings in the step S1;
s3, carrying out four times of concentration on the rough concentrate obtained in the step S1 to obtain the concentrate containing the rare earth component.
7. The method for recovering rare earth components from waste polishing powder according to claim 6, wherein in step S1, the roughing recipe is: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.8-2.2 kg/t, the addition amount of the collector relative to the raw ore is 1.8-2.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.15-0.25 kg/t.
8. The method for recycling rare earth components from waste polishing powder according to claim 6, wherein in step S2, the first scavenging and the second scavenging require the addition of a chemical, and the third scavenging does not require the addition of a chemical; the medicament system for the first scavenging is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.0-1.4 kg/t, the addition amount of the collector relative to the raw ore is 1.2-1.6 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.08-0.1 kg/t; the second scavenging medicament system is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 0.8-1.0 kg/t, the addition amount of the collector relative to the raw ore is 1.0-1.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.05-0.08 kg/t.
9. The method for recovering rare earth elements from waste polishing powder as claimed in claim 6, wherein in step S3, the first to third concentration requires the addition of chemicals, the fourth concentration requires no addition of chemicals, and the first concentration has a chemical system of: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.4-1.8 kg/t, the addition amount of the collector relative to the raw ore is 1.6-2.0 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.1-0.2 kg/t; the second selection is carried out according to the following medicament system: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 1.0-1.4 kg/t, the addition amount of the collector relative to the raw ore is 1.2-1.5 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.09-0.12 kg/t; the third selection medicament system is as follows: adding a pH regulator to regulate the pH of the ore pulp to 2.5-3.5; the addition amount of the inhibitor relative to the raw ore is 0.8-1.0 kg/t, the addition amount of the collector relative to the raw ore is 1.0-1.2 kg/t, and the addition amount of the foaming agent relative to the raw ore is 0.05-0.08 kg/t.
10. The method for recovering rare earth components from waste polishing powder as set forth in claim 6, wherein in the steps S2 and S3, the coarse middlings obtained in the scavenging process are returned to the upper stage flotation as a feed; the fine middlings obtained in the concentration process are returned to the last stage of flotation as feed.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4389292A1 (en) * | 2022-12-20 | 2024-06-26 | ArrMaz Products Inc. | Collector composition for rare earth ore beneficiation |
| EP4389291A1 (en) * | 2022-12-20 | 2024-06-26 | ArrMaz Products Inc. | Collector composition for lithium ore beneficiation |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274796A (en) * | 2011-07-28 | 2011-12-14 | 内蒙古科技大学 | Beneficiation method for purifying bastnaesite concentrate |
| CN102319631A (en) * | 2011-07-28 | 2012-01-18 | 内蒙古科技大学 | A kind of from the Bayan Obo mine tailing method of flotation rare earth |
| CN102886308A (en) * | 2012-10-15 | 2013-01-23 | 内蒙古科技大学 | Method for recycling waste rare-earth polishing powder |
| CN102886312A (en) * | 2012-10-15 | 2013-01-23 | 内蒙古科技大学 | Mineral sorting method for separating bastnaesite and monazite from high-grade mixed rare-earth concentrate |
| CN104087757A (en) * | 2014-07-12 | 2014-10-08 | 连云港健发磁性材料有限公司 | Simplified method for recovering rare earth elements from waste residues of rare earth polishing powder |
| CN106563561A (en) * | 2016-08-31 | 2017-04-19 | 李梅 | Method of improving rare earth grade of hybrid rare earth ores |
| KR101766788B1 (en) * | 2017-01-12 | 2017-08-11 | 대한민국 | Method of Separating Rare Earth Elements From Rare Earth Polishing Power Wastes |
| GB201809818D0 (en) * | 2018-06-15 | 2018-08-01 | Seren Tech Limited | Countercurrent rare earth separation process |
| CN108359408A (en) * | 2017-01-26 | 2018-08-03 | 新岛世纪（北京）新型材料技术有限公司 | A method of recycling polishing powder from polishing powder from rare earth waste residue |
| CN114107668A (en) * | 2021-11-10 | 2022-03-01 | 北京工业大学 | Method for mechanically activating and strengthening leaching rare earth in waste polishing solution |
-
2022
- 2022-03-21 CN CN202210279767.7A patent/CN114700180B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102274796A (en) * | 2011-07-28 | 2011-12-14 | 内蒙古科技大学 | Beneficiation method for purifying bastnaesite concentrate |
| CN102319631A (en) * | 2011-07-28 | 2012-01-18 | 内蒙古科技大学 | A kind of from the Bayan Obo mine tailing method of flotation rare earth |
| CN102886308A (en) * | 2012-10-15 | 2013-01-23 | 内蒙古科技大学 | Method for recycling waste rare-earth polishing powder |
| CN102886312A (en) * | 2012-10-15 | 2013-01-23 | 内蒙古科技大学 | Mineral sorting method for separating bastnaesite and monazite from high-grade mixed rare-earth concentrate |
| CN104087757A (en) * | 2014-07-12 | 2014-10-08 | 连云港健发磁性材料有限公司 | Simplified method for recovering rare earth elements from waste residues of rare earth polishing powder |
| CN106563561A (en) * | 2016-08-31 | 2017-04-19 | 李梅 | Method of improving rare earth grade of hybrid rare earth ores |
| KR101766788B1 (en) * | 2017-01-12 | 2017-08-11 | 대한민국 | Method of Separating Rare Earth Elements From Rare Earth Polishing Power Wastes |
| CN108359408A (en) * | 2017-01-26 | 2018-08-03 | 新岛世纪（北京）新型材料技术有限公司 | A method of recycling polishing powder from polishing powder from rare earth waste residue |
| GB201809818D0 (en) * | 2018-06-15 | 2018-08-01 | Seren Tech Limited | Countercurrent rare earth separation process |
| CN114107668A (en) * | 2021-11-10 | 2022-03-01 | 北京工业大学 | Method for mechanically activating and strengthening leaching rare earth in waste polishing solution |
Non-Patent Citations (3)
| Title |
|---|
| 孙传尧等: "《选矿工程师手册》", 31 March 2015, pages: 289 - 291 * |
| 曾小波等: "某极低品位稀土矿选矿提纯试验研究", 《矿产综合利用》 * |
| 曾小波等: "某极低品位稀土矿选矿提纯试验研究", 《矿产综合利用》, no. 06, 25 December 2014 (2014-12-25), pages 32 - 34 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4389292A1 (en) * | 2022-12-20 | 2024-06-26 | ArrMaz Products Inc. | Collector composition for rare earth ore beneficiation |
| EP4389291A1 (en) * | 2022-12-20 | 2024-06-26 | ArrMaz Products Inc. | Collector composition for lithium ore beneficiation |
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