CN115820130A - Regeneration method of rare earth polishing powder - Google Patents
Regeneration method of rare earth polishing powder Download PDFInfo
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- CN115820130A CN115820130A CN202310013119.1A CN202310013119A CN115820130A CN 115820130 A CN115820130 A CN 115820130A CN 202310013119 A CN202310013119 A CN 202310013119A CN 115820130 A CN115820130 A CN 115820130A
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- rare earth
- solid product
- polishing powder
- alkali liquor
- earth polishing
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 102
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 102
- 238000005498 polishing Methods 0.000 title claims abstract description 85
- 239000000843 powder Substances 0.000 title claims abstract description 80
- 238000011069 regeneration method Methods 0.000 title claims abstract description 30
- 239000012265 solid product Substances 0.000 claims abstract description 66
- 239000003513 alkali Substances 0.000 claims abstract description 53
- 239000002699 waste material Substances 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 30
- 239000000126 substance Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000005201 scrubbing Methods 0.000 claims description 35
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 33
- 239000002002 slurry Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 23
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000011084 recovery Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 239000011268 mixed slurry Substances 0.000 description 8
- 239000012065 filter cake Substances 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000003682 fluorination reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910001854 alkali hydroxide Inorganic materials 0.000 description 2
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical group [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 238000007517 polishing process Methods 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000010902 jet-milling Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a regeneration method of rare earth polishing powder. The regeneration method comprises the following steps: (1) Reacting the rare earth polishing powder waste from which the large-particle impurities are removed with a first alkali liquor to obtain a first solid product; wherein the particle size of the large-particle impurities is more than or equal to 60 meshes, and the concentration of the first alkali liquor is 50-300 g/L; (2) Reacting the first solid product with a second alkali liquor to obtain a second solid product; wherein the concentration of the second alkali liquor is 200-600 g/L, and the concentration of the second alkali liquor is greater than that of the first alkali liquor; (3) Fluorinating the second solid product to obtain a third solid product; and (4) roasting the third solid product. The method can effectively reduce the consumption of alkaline substances.
Description
Technical Field
The invention relates to a regeneration method of rare earth polishing powder.
Background
The main component of the rare earth polishing powder is cerium oxide, which can rapidly polish optical glass. In the polishing process, the shape and the granularity of the rare earth polishing powder crystal grains are continuously changed, edges and corners are gradually ground off and become similar to spherical shapes, the granularity is gradually reduced, and the polishing capability is lost. Meanwhile, a large amount of glass powder particles are enriched on the surface of the rare earth polishing powder in the polishing process, and in addition, oil stains and large particle foreign matters are continuously mixed, so that the close contact between the glass surface and the polishing powder particles is hindered, and the rare earth polishing powder loses the polishing capability. In recent years, as the demand of consumers for electronic products is increasing, the usage amount of rare earth polishing powder is also increasing year by year. If these waste rare earth polishing powders are directly discarded, a huge loss is caused. How to regenerate the waste rare earth polishing powder at low cost becomes an urgent problem to be solved.
CN102167956A discloses a method for recovering waste residue and waste liquid of rare earth polishing powder. The method comprises the steps of removing impurities of polishing powder waste liquid in a high-speed dispersion machine or a vibrating screen for one time; pouring the polishing powder waste liquid subjected to primary impurity removal into a centrifuge for secondary impurity removal; carrying out filter pressing treatment on the waste polishing powder subjected to secondary impurity removal to obtain waste polishing powder mud blocks subjected to tertiary impurity removal; dispersing the waste polishing powder mud blocks by a high-speed dispersion machine, and then screening by a vibrating screen to obtain a concentrated polishing agent; and adding water to dilute the concentrated polishing agent to obtain a recovered rare earth polishing agent finished product. The rare earth polishing agent obtained by the method has low rare earth grade.
CN 103215012A discloses a preparation method for regeneration of rare earth polishing powder. The method comprises the steps of mixing waste rare earth polishing powder, adopting table concentrator gravity separation equipment for gravity separation, separating heavy components, and drying to obtain gravity separation rare earth polishing powder; treating the gravity rare earth polishing powder with an ammonium hexafluorozirconate aqueous solution, then settling, and recovering solids to obtain primary rare earth polishing powder; and (3) primarily drying the primary rare earth polishing powder, and then roasting, cooling, jet milling and the like to obtain the regenerated rare earth polishing powder. The method needs ammonium hexafluorozirconate, and has high cost.
CN1456624A discloses a regeneration method of spent rare earth polishing powder. The method comprises the steps of chemically treating chemical reagents containing water-soluble alkali and water-soluble fluoride with certain concentration in ineffective rare earth polishing powder slurry, heating and stirring for a certain time, and then recovering solids through sedimentation, cleaning and filtration; the recovered solid was further heat-treated and then cooled to room temperature. The method has the advantages of large consumption of alkaline substances and fluoride and high cost.
Disclosure of Invention
In view of the above, the present invention provides a method for regenerating rare earth polishing powder, which can effectively reduce the amount of alkaline substances and the production cost. Furthermore, the method can obtain the regenerated rare earth polishing powder with higher rare earth grade, and the recovery rate of the rare earth is higher. The above object is achieved by the following technical solutions.
The invention provides a regeneration method of rare earth polishing powder, which comprises the following steps:
(1) Reacting the rare earth polishing powder waste from which the large-particle impurities are removed with a first alkali liquor to obtain a first solid product; wherein the particle size of the large-particle impurities is more than or equal to 60 meshes, and the concentration of the first alkali liquor is 50-250 g/L;
(2) Reacting the first solid product with a second alkali liquor to obtain a second solid product; wherein the concentration of the second alkali liquor is 200-600 g/L, and the concentration of the second alkali liquor is greater than that of the first alkali liquor;
(3) Fluorinating the second solid product to obtain a third solid product;
(4) And roasting the third solid product.
According to the regeneration method, the weight ratio of the first alkali liquor to the rare earth polishing powder waste material for removing large-particle impurities is preferably (3-15): 1; the weight ratio of the second alkali liquor to the first solid product is (3-15) to 1.
According to the regeneration method of the present invention, preferably, in the step (1), the rare earth polishing powder waste material from which the large particle impurities are removed is reacted with the first alkali solution at 50 to 150 ℃ for 10 to 200min; in the step (2), the first solid product and the second alkali liquor react for 10-800 min at 100-350 ℃.
According to the regeneration method of the present invention, preferably, the alkaline substance in the first alkali liquor is a water-soluble hydroxide, and the alkaline substance in the second alkali liquor is a water-soluble hydroxide.
According to the regeneration method of the present invention, preferably, in the step (3), the second solid product is reacted with fluoride to obtain a third solid product; wherein the fluoride is selected from one or more of hydrofluoric acid or ammonium fluoride.
According to the regeneration method of the invention, preferably, the reaction temperature of the second solid product and the fluoride is 20-120 ℃, and the reaction time is 10-300 min; the second solid product is used in the form of slurry, and the concentration of the slurry of the second solid product is 10-80 wt%; the fluoride is used in the form of an aqueous solution, the concentration of the aqueous fluoride solution is 4-50 wt%, and the mass of the aqueous fluoride solution is 3-10 wt% of the mass of the rare earth oxide in the second solid product.
According to the regeneration method of the present invention, it is preferable that the calcination temperature is 700 to 1100 ℃ and the calcination time is 100 to 700min.
The regeneration method according to the present invention preferably further comprises the steps of:
scrubbing the rare earth polishing powder waste to obtain scrubbing slurry; and sieving the scrubbing slurry, and then filtering the sieved substances to obtain the rare earth polishing powder waste material without large-particle impurities.
According to the regeneration method of the invention, the rare earth grade of the rare earth polishing powder waste is preferably more than or equal to 65wt%.
The regeneration method according to the present invention preferably further comprises the steps of: and crushing the roasted product to obtain the regenerated rare earth polishing powder.
The method can reduce the use amount of alkaline substances and the regeneration cost of the rare earth polishing powder, and has great economic value. The method ensures that the obtained regenerated rare earth polishing powder has higher rare earth grade and higher rare earth recovery rate through the mutual matching of the steps.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
The method adopts the low-concentration alkali liquor to remove silicon-aluminum impurities in the rare earth polishing powder waste, and adopts the high-concentration alkali liquor to realize crystal reconstruction and phase regeneration of the rare earth polishing powder waste, so that the use amount of alkaline substances can be reduced, and the cost is reduced. The alkali liquor with high concentration after the reaction can be recycled and used as raw materials, thereby further reducing the production cost. In addition, the regeneration method of the invention uses less fluoride in the fluorination step.
The regeneration method of the rare earth polishing powder comprises the following steps: (1) a step of physical screening; (2) a step of primary alkali liquor treatment; (3) a second alkali liquor treatment step; (4) a fluorination step; (5) a step of roasting; and (6) a step of pulverizing. As described in detail below.
Step of physical sieving
Scrubbing the rare earth polishing powder waste to obtain scrubbing slurry; and sieving the scrubbing slurry, and then filtering the sieved substances to obtain the rare earth polishing powder waste material without large-particle impurities.
The rare earth grade of the rare earth polishing powder waste is more than or equal to 65wt%; preferably, the rare earth grade of the rare earth polishing powder waste is more than or equal to 70wt%; more preferably, the rare earth grade of the rare earth polishing powder waste is 70-85 wt%.
The aperture of the screen mesh can be 60-500 meshes. In some embodiments, the mesh has a mesh size of 80 to 400 mesh. In other embodiments, the mesh has a mesh size of 300 to 400 mesh. Thus, the consumption of alkaline substances can be reduced, and the rare earth grade and the rare earth recovery rate of the regenerated rare earth polishing powder are improved.
The concentration of the mixed slurry can be 30-90 wt%; preferably 40 to 80wt%; more preferably 50 to 70wt%.
The scrubbing temperature can be 10-80 ℃; preferably 20 to 70 ℃; more preferably 30 to 60 ℃.
The total scrubbing time can be 10-100 min; preferably 20 to 90min.
According to one embodiment of the invention, a first mixed slurry of rare earth polishing powder waste and water is subjected to primary scrubbing in a scrubbing tank to obtain a first scrubbing slurry. And sieving the first scrubbing slurry to obtain a first-stage oversize product and a first-stage undersize product. And carrying out secondary scrubbing on second mixed slurry formed by the primary oversize products and water in the scrubbing tank to obtain second scrubbing slurry. And sieving the second scrubbing slurry to obtain a second-level oversize product and a second-level undersize product. And filtering the primary undersize product and the secondary undersize product to obtain the rare earth polishing powder waste from which large-particle impurities are removed.
The mesh size used for the first scrubbing slurry screening may or may not be the same as the mesh size used for the second scrubbing slurry screening. The mesh openings are in particular as described above.
The concentration of the first mixed slurry and the concentration of the second mixed slurry may be the same or different. The concentration of the mixed slurry is specifically as described above.
The primary scrubbing temperature and the secondary scrubbing temperature may or may not be the same. The scrub temperature is as described above.
The primary scrubbing time may or may not be the same as the secondary scrubbing time. The primary scrubbing time can be 5-70 min; preferably 10 to 60min. The secondary scrubbing time can be 5-70 min; preferably 10 to 60min.
Step of primary alkali solution treatment
And reacting the rare earth polishing powder waste from which the large-particle impurities are removed with a first alkali liquor to obtain a first solid product. Specifically, a first reactant obtained by reacting the rare earth polishing powder waste from which the large-particle impurities are removed with a first alkali solution is filtered to obtain a first solid product.
The particle size of the large-particle impurities is more than or equal to 60 meshes. In some embodiments, the large particle impurities have a particle size of 80 mesh or larger. In other embodiments, the large particle impurities have a particle size of 400 mesh or larger. Impurities refer to non-rare earth species other than rare earth oxides.
The alkaline substance in the first alkali liquor can be water-soluble hydroxide; aqueous alkali or alkaline earth metal hydroxides are preferred. Examples of alkaline materials include, but are not limited to, sodium hydroxide, potassium hydroxide.
The concentration of the first alkali liquor is 50-250 g/L; preferably 60 to 200g/L; more preferably 80 to 100g/L. Thus, the consumption of alkaline substances can be reduced, and the rare earth grade and the rare earth recovery rate of the regenerated rare earth polishing powder are improved.
The mass ratio of the rare earth polishing powder without large particle impurities to the first alkali liquor can be 1 (3-15); preferably 1 (4-12); more preferably 1 (5-10).
The rare earth polishing powder waste material from which the large-particle impurities are removed and the first alkali solution can react under the condition of stirring. The reaction temperature can be 50-150 ℃; preferably 60 to 100 ℃; more preferably 70 to 90 deg.c. The reaction time can be 10-200 min; preferably 30-150 min; more preferably 50 to 100min.
Second alkali solution treatment step
And reacting the first solid product with a second alkali liquor to obtain a second solid product. Specifically, a second reactant obtained by reacting the first solid product with a second alkaline solution is filtered to obtain a filtrate and a filter cake. And washing the filter cake to obtain a second solid product. Specifically, mixing a filter cake with water, and stirring and washing to ensure that the pH of slurry formed by the filter cake and the water is less than 10; the slurry was then filtered to give a second solid product. The filtrate can be used as a raw material for preparing the first slurry and the second slurry. This can reduce the amount of alkaline substances used.
The alkaline substance in the second alkali liquor can be water-soluble hydroxide; preferably an aqueous alkali or alkaline earth metal hydroxide. Examples of alkaline materials include, but are not limited to, sodium hydroxide, potassium hydroxide.
The concentration of the second alkali liquor is greater than that of the first alkali liquor. The concentration of the second alkali liquor is 200-600 g/L; preferably 250 to 500g/L; more preferably 300 to 400g/L. Thus, the consumption of alkaline substances can be reduced, and the rare earth grade and the rare earth recovery rate of the regenerated rare earth polishing powder are improved.
The mass ratio of the first solid product to the second alkali liquor can be 1 (3-15); preferably 1 (4-12); more preferably 1 (5-10).
The first solid product can be reacted with the second alkali liquor under stirring. The reaction temperature can be 100-350 ℃; preferably 150 to 300 ℃; more preferably from 200 to 250 ℃. The reaction time can be 10-800 min; preferably 50-700 min; more preferably 100 to 600min.
Step of fluorination
And fluorinating the second solid product to obtain a third solid product. Specifically, a third reaction product obtained by fluorinating the second solid product is filtered and then dried to obtain a third solid product.
The second solid product is reacted with a fluoride. The fluoride may be hydrogen fluoride and ammonium fluoride. The amount of fluoride in the second solid product may be 0.1-5 wt% of the rare earth oxide; preferably 0.5 to 3.5wt%; more preferably 2 to 3.5wt%. The fluoride may be used in the form of an aqueous solution thereof. The concentration of the aqueous fluoride solution may be 4 to 50wt%; preferably 10 to 40wt%. The using amount of the fluoride aqueous solution accounts for 3-10 wt% of the rare earth oxide in the second solid product; preferably 5 to 8wt%. Thus, the consumption of fluoride can be reduced, and the rare earth grade and the rare earth recovery rate of the regenerated rare earth polishing powder are improved.
The second solid product may be used in the form of a slurry. The concentration of the second solid product slurry is 10-80 wt%; preferably 20 to 70wt%; more preferably 30 to 60wt%.
The reaction temperature of the second solid product and fluoride is 20-120 ℃; preferably 40 to 100 ℃; more preferably 50 to 80 ℃. Thus, the consumption of fluoride can be reduced, and the rare earth grade and the rare earth recovery rate of the regenerated rare earth polishing powder are improved.
The reaction time of the second solid product and fluoride is 10-300 min; preferably 30-200 min; more preferably 30 to 100min.
According to one embodiment of the invention, an aqueous fluoride solution is added to the stirring second solid product slurry. The aqueous fluoride solution is added into the aqueous fluoride solution within 30-150 min. Preferably, the aqueous fluoride solution is added to the aqueous fluoride solution within 60 to 120 min. Adding the fluoride aqueous solution into the fluoride aqueous solution at a constant speed. The temperature of the fluoride water solution is 20-120 ℃; preferably 40 to 100 ℃; more preferably 50 to 80 ℃.
The drying temperature can be 60-200 ℃; preferably 80 to 150 ℃; more preferably 100 to 120 ℃.
The water content in the third solid product was < 1wt%.
Step of calcination
And roasting the third solid product.
The roasting temperature is 700-1100 ℃; preferably 800-1000 ℃; more preferably 900 to 950 ℃.
The roasting time is 100-700 min; preferably 300-600 min; more preferably 300 to 500min.
A step of pulverizing
And crushing the roasted product to obtain the regenerated rare earth polishing powder. The method of pulverization may employ a method commonly used in the art, for example, jet pulverization of the calcined product. And classifying the crushed roasted product to obtain the regenerated rare earth polishing powder with a certain particle size.
The following describes the test and calculation methods:
rare earth grade: according to GB/T20166.1-2012 rare earth polishing powder chemical analysis method: measurement of the amount of cerium oxide was determined by titration.
The rare earth recovery rate calculation method comprises the following steps:
rare earth recovery rate = (rare earth grade in recycled rare earth polishing powder x recycled rare earth polishing powder quality)/(rare earth grade in rare earth polishing powder waste x rare earth polishing powder waste quality)
Examples 1 to 2
And performing primary scrubbing on first mixed slurry formed by the rare earth polishing powder waste and water in a scrubbing tank to obtain first scrubbing slurry. And sieving the first scrubbing slurry to obtain a first-stage oversize product and a first-stage undersize product. And carrying out secondary scrubbing on second mixed slurry formed by the primary oversize products and water in the scrubbing tank to obtain second scrubbing slurry. And sieving the second scrubbing slurry to obtain a second grade oversize product and a second grade undersize product. And filtering the primary undersize product and the secondary undersize product to obtain the rare earth polishing powder waste from which large-particle impurities are removed.
Stirring the rare earth polishing powder waste material without large-particle impurities and a first sodium hydroxide solution at T 1 Reaction at temperature t 1 And (4) obtaining a first reactant. The first reactant is filtered to yield a first solid product.
Mixing the first solid product with a second sodium hydroxide solution under stirring at T 2 Reaction at temperature t 2 And (4) obtaining a second reactant. The second reactant is filtered to obtain a filter cake and a filtrate. Mixing the filter cake with water, and stirring and washing to ensure that the pH of slurry formed by the filter cake and the water is less than 10; the slurry was then filtered to give a second solid product. The filtrate can be used as a raw material for preparing the first sodium hydroxide solution and the second sodium hydroxide solution.
The second solid product is combined with water to form a second solid product slurry. At T 3 At temperature and t 3 And adding hydrofluoric acid into the stirred second solid product slurry at a constant speed within the time. After the hydrofluoric acid is completely added, the hydrofluoric acid and the second solid product slurry are reacted under the condition of stirring 4 And (4) obtaining a third reaction product. And filtering the third reaction product, and drying at 100 ℃ to obtain a third solid product with the water content of less than 1wt%.
And roasting the third solid product to obtain a roasted product.
And (3) airflow crushing and grading the roasted product to obtain the regenerated rare earth polishing powder.
Specific parameters are shown in table 1. The properties and rare earth recovery rates of the obtained regenerated rare earth polishing powders are shown in Table 1.
TABLE 1
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (10)
1. A regeneration method of rare earth polishing powder is characterized by comprising the following steps:
(1) Reacting the rare earth polishing powder waste material without large-particle impurities with a first alkali liquor to obtain a first solid product; wherein the particle size of the large-particle impurities is more than or equal to 60 meshes, and the concentration of the first alkali liquor is 50-250 g/L;
(2) Reacting the first solid product with a second alkali liquor to obtain a second solid product; wherein the concentration of the second alkali liquor is 200-600 g/L, and the concentration of the second alkali liquor is greater than that of the first alkali liquor;
(3) Fluorinating the second solid product to obtain a third solid product;
(4) And roasting the third solid product.
2. The regeneration method of claim 1, wherein the weight ratio of the first alkali solution to the rare earth polishing powder waste material from which the large-particle impurities are removed is (3-15): 1; the weight ratio of the second alkali liquor to the first solid product is (3-15) to 1.
3. The regeneration method according to claim 1, characterized in that:
in the step (1), the rare earth polishing powder waste material without large particle impurities reacts with first alkali liquor for 10-200 min at 50-150 ℃;
in the step (2), the first solid product and the second alkali liquor react for 10-800 min at 100-350 ℃.
4. The regeneration method of claim 1, wherein the alkaline substance in the first alkali solution is a water-soluble hydroxide, and the alkaline substance in the second alkali solution is a water-soluble hydroxide.
5. The regeneration process of claim 1, wherein in step (3), the second solid product is reacted with fluoride to produce a third solid product;
wherein the fluoride is selected from one or more of hydrofluoric acid or ammonium fluoride.
6. The regeneration method according to claim 5, characterized in that:
the reaction temperature of the second solid product and fluoride is 20-120 ℃, and the reaction time is 10-300 min;
the second solid product is used in the form of slurry, and the concentration of the slurry of the second solid product is 10-80 wt%;
the fluoride is used in the form of an aqueous solution, the concentration of the aqueous fluoride solution is 4-50 wt%, and the mass of the aqueous fluoride solution is 3-10 wt% of the mass of the rare earth oxide in the second solid product.
7. The regeneration method according to claim 1, wherein the calcination temperature is 700 to 1100 ℃ and the calcination time is 100 to 700min.
8. The regeneration method according to claim 1, further comprising the steps of:
scrubbing the rare earth polishing powder waste to obtain scrubbing slurry; and sieving the scrubbing slurry, and then filtering the sieved substances to obtain the rare earth polishing powder waste material without large-particle impurities.
9. The recycling method according to claim 1, wherein the rare earth grade of the rare earth polishing powder waste is not less than 65wt%.
10. The regeneration method according to any one of claims 1 to 9, further comprising the steps of:
and crushing the roasted product to obtain the regenerated rare earth polishing powder.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1190825A (en) * | 1997-09-18 | 1999-04-06 | Fukushima Prefecture | Polishing material recovering method |
| CN1456624A (en) * | 2003-03-10 | 2003-11-19 | 田汝梅 | Fail rare earth polishing powder reproducing method |
| CN103215012A (en) * | 2013-04-26 | 2013-07-24 | 济南大学 | Preparation method for regenerating rear-earth polishing powder |
| JP2015533660A (en) * | 2012-09-14 | 2015-11-26 | エルジー・ケム・リミテッド | Recycling method of waste abrasive containing ceria |
| CN107129761A (en) * | 2017-04-25 | 2017-09-05 | 中国环境科学研究院 | The method of sial impurity in the discarded polishing powder of removing |
| CN114213976A (en) * | 2021-12-14 | 2022-03-22 | 甘肃金阳高科技材料有限公司 | Method for preparing rare earth polishing powder for cover plate glass by using glass polishing waste residue particle regeneration technology |
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2023
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1190825A (en) * | 1997-09-18 | 1999-04-06 | Fukushima Prefecture | Polishing material recovering method |
| CN1456624A (en) * | 2003-03-10 | 2003-11-19 | 田汝梅 | Fail rare earth polishing powder reproducing method |
| JP2015533660A (en) * | 2012-09-14 | 2015-11-26 | エルジー・ケム・リミテッド | Recycling method of waste abrasive containing ceria |
| CN103215012A (en) * | 2013-04-26 | 2013-07-24 | 济南大学 | Preparation method for regenerating rear-earth polishing powder |
| CN107129761A (en) * | 2017-04-25 | 2017-09-05 | 中国环境科学研究院 | The method of sial impurity in the discarded polishing powder of removing |
| CN114213976A (en) * | 2021-12-14 | 2022-03-22 | 甘肃金阳高科技材料有限公司 | Method for preparing rare earth polishing powder for cover plate glass by using glass polishing waste residue particle regeneration technology |
Non-Patent Citations (2)
| Title |
|---|
| 史培阳;王希鑫;丁文清;李鑫哲;: "废弃稀土抛光粉资源化利用研究现状", 资源节约与环保, no. 01 * |
| 罗天纵;吴希桃;包新军;王志坚;夏楚平;兰石琨;翁国庆;陈建波;: "废弃稀土抛光粉回收再利用研究进展", 稀土, no. 03 * |
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