CN104962200A - Recovery preparation method of waste rare-earth polishing powder - Google Patents
Recovery preparation method of waste rare-earth polishing powder Download PDFInfo
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- CN104962200A CN104962200A CN201510437815.0A CN201510437815A CN104962200A CN 104962200 A CN104962200 A CN 104962200A CN 201510437815 A CN201510437815 A CN 201510437815A CN 104962200 A CN104962200 A CN 104962200A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention discloses a recovery preparation method of waste rare-earth polishing powder, which comprises the following steps: 1. adding a certain amount of water into waste rare-earth polishing powder, immersing for 1.5-2.5 hours, sequentially screening the filtrate through a 50-100-mesh screen and a 500-1000-mesh screen, precipitating the filtrate, and drying at 180-220 DEG C to obtain purified waste rare-earth polishing powder; 2. weighing 100 parts of purified waste rare-earth polishing powder, 1-5 parts of additive I and 5-15 parts of additive II, uniformly mixing, and grinding for 5-30 minutes, wherein the additive I is ammonium sulfate, and the additive II is silicon dioxide; 3. adding the ground material into a tank, roasting in a furnace at 700-1000 DEG C for 2-6 hours, naturally cooling in the furnace, opening the furnace door, and taking out; and 4. carrying out ball milling on the material to the required particle size, drying and bagging. The method for recovering the waste polishing powder by adding the additives has the advantages of simple technique, low production cost, high recovery efficiency and favorable comprehensive properties of the recovered polishing powder, and maximally reduces the environmental pollution in the whole recovery process.
Description
Technical field
The present invention relates to the reclaiming method of waste and old polishing powder from rare earth, belong to technical field of resource comprehensive utilization, be specifically related to a kind of preparation method for the waste and old polishing powder from rare earth reclaiming after use in optics, electron trade.
Background technology
China is the country that a rare earth resources enriches, Rare Earth Production amount is maximum, polishing powder from rare earth is as a product very important in all kinds of rare-earth products, its output in all kinds of rare-earth products is maximum, and China's annual production reaches 100,000 tons, for domestic year usage quantity about 30,000 tons.And if polishing powder from rare earth is direct as waste discharge after a procedure, to unavoidably cause serious environmental pollution, also be waste the one of rare earth resources, therefore recycle very necessary to the waste and old polishing powder from rare earth after use, it can produce obvious economic and social benefit simultaneously.
Past is for the reclaiming technique of waste and old polishing powder from rare earth, major part adopts acid-soluble method, as the Chinese invention patent " renovation process of inefficacy polishing powder " that Chinese invention patent " regenerates the preparation method of polishing powder from rare earth ", the patent No. is CN03119524.5 that the patent No. is CN03130446.X, and the patent No. is the Chinese invention patent " a kind of regeneration is applied to the method for the discarded polishing powder from rare earth of crystal glass " of CN201110265136, it is complex process but also big for environment pollution not only, and process costs is also high simultaneously.To this, need a kind of gradual changed method of acid dissolve that do not use badly to realize the regeneration of waste and old polishing powder from rare earth.
Although in the reclaiming method of existing waste and old polishing powder from rare earth, also the method adopting and add the Ficus caricaL of oxygenatedchemicals is had, as the Chinese invention patent " a kind of preparation method of polishing powder from rare earth regeneration " that the patent No. is CN201310148306.7, but but there is the problem of wastewater treatment in it.
Summary of the invention
For overcoming above-mentioned prior art defect, the object of the present invention is to provide a kind of reclaiming novel method of waste and old polishing powder from rare earth, it is by adding additive mixing after carrying out purification to waste and old polishing powder from rare earth, grinding and bake, generate new polishing powder from rare earth, realize effectively carrying out on the basis of reclaiming to waste and old polishing powder from rare earth, no longer produce new environmental pollution, and easy and simple to handle.
For realizing above-mentioned technical purpose, the present invention takes following technical scheme:
A kind of waste and old polishing powder from rare earth reclaiming preparation method, is characterized in that, comprise the following steps:
1, the purification of waste and old polishing powder from rare earth
Waste and old polishing powder from rare earth is soaked, is cleaned by 1.1, and the mass ratio of water and waste and old polishing powder from rare earth is 4:1, soak time 1.5-2.5 hour;
1.2 to sieve process to the mixed solution in step 1.1 with 50-100 object screen cloth, the large granular impurity in removing mixed solution;
1.3 to sieve process to the filtrate in step 1.2 with 500-1000 object screen cloth, and liquid precipitate post-drying to be filtered, bake out temperature 180-220 DEG C, obtains the waste and old polishing powder from rare earth of purification.
2, the selection of additive
2.1 prepare additive I: be ammonium sulfate, level Four reagent;
2.2 prepare additive II: be silicon-dioxide, pale powder.
3, waste and old polishing powder from rare earth is with the proportioning of additive
Waste and old polishing powder from rare earth after purification mixes by following mass ratio with additive by 3.1:
Discarded polishing powder from rare earth after purification: 100 parts, additive I:1-5 part, additive II:5-15 part, also can add appropriate pure zirconia cerium powder according to specific requirement;
Wherein, the Main Function of additive I and additive II is the reaction of oxidation-reduction reaction Sum decomposition, realizes the reunion reducing powder in the process of roasting, obtains spheroidal particle, reduces the color and luster of powder simultaneously, improves sponginess;
3.2 by mixed for step 3.1 material milling apparatus grinding 5-30 minute;
4, the roasting regeneration of waste and old polishing powder from rare earth
4.1 step 3.2 is ground after material tinning, at kiln roasting, maturing temperature 700-1000 DEG C, roasting time 2-6 hour;
After 4.2 power-off, allow material naturally cool to less than 300 DEG C with stove, blow-on goalkeeper material takes out;
Material after 4.3 pairs of step 4.2 roastings carries out ball milling, is milled to desired particle size;
Material after step 4.3 ball milling carries out drying, packing by 4.4.
By above technical scheme, advantage of the present invention and beneficial effect are:
1, adopt the method adding additive, waste and old polishing powder is regenerated, has the advantages that technique is simple, production cost is low, organic efficiency is high;
2, the polishing powder good combination property of regeneration, has good suspension, is applicable to the polishing requirement of different class;
3, whole reclaiming process only produces few waste gas, but configurable gas absorbing device processes, and decreases the pollution to environment to greatest extent.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but not as a limitation of the invention.
Embodiment 1
Waste and old high-cerium rare-earth polishing powder after the present embodiment uses with optical manufacturing factory polishing departement is for raw material, and concrete steps are as follows:
1, by waste and old polishing powder from rare earth and water in mass ratio 1:4 mix and soak, soak time 1.5 hours;
2, the mixed solution in step 1 is filtered and 500 object fine screen mesh filtration treatment through 50 object wide-meshed screens successively, remove the impurity that in mixed solution, particle is larger;
3, dry after the filtrate precipitation of step 2, bake out temperature 180-200 DEG C, completes the purification of waste and old polishing powder from rare earth;
4, the waste and old polishing powder after step 3 purification is carried out to the mensuration of content of rare earth and cerium-oxide contents, its Rare-Earth Content is 95.10%, and cerium-oxide contents is 70.20%;
5, the waste and old polishing powder from rare earth after purification described in step 4 is taken: 1000g, mix together with additive I:30g, additive II:85g and grind with steel mill, milling time 7 minutes, wherein additive I is ammonium sulfate, level Four reagent, additive II main component is silicon-dioxide, provides for Suzhou Na Fang engineering materials company limited produces;
6, the material after step 5 being ground is loaded in porcelain dish, puts into the roasting of retort furnace mouth, continuous warming to 900 DEG C, and soaking time power-off after 3 hours, makes material naturally cool to room temperature with stove, is milled to particle diameter about 2.0 μm after taking-up with ball mill;
7, the material after step 6 ball milling is dried, packed.
Embodiment 2
Waste and old high-cerium rare-earth polishing powder after the present embodiment uses with optical manufacturing factory polishing departement is for raw material, and concrete steps are as follows:
1, make waste and old polishing powder from rare earth and water in mass ratio 1:4 mix and soak, soak 1.8 hours;
2, the mixed solution in step 1 is filtered and 700 object fine screen mesh filtration treatment through 70 object wide-meshed screens successively, remove the impurity that particle is larger;
3, dry after the filtrate precipitation in step 2, bake out temperature 200 DEG C, obtaining outward appearance is baby pink powder, realizes the purification of waste and old polishing powder from rare earth;
4, the waste and old polishing powder after step 3 purification is carried out to mensuration and the dynamics mensuration of content of rare earth and cerium-oxide contents, record particle diameter D50=1.45 μm;
5, take the waste and old polishing powder from rare earth after purification described in step 4: 450g, mix together with additive I:12g, additive II:80g, grind in agate mortar by hand, milling time 18 minutes, wherein additive I is ammonium sulfate, level Four reagent, and additive II is silicon-dioxide;
6, the material after step 5 being ground is loaded in porcelain crucible, material brim height is the 2/3-3/4 of porcelain crucible height, recessed in the middle part of material, put into the roasting of retort furnace mouth, continuous warming to 930 DEG C, soaking time power-off after 4 hours, makes material naturally cool to room temperature with stove, take out and survey particle diameter, D90=15.28 μm, D50=8.27 μm;
7, carry out ball milling to material, Ball-milling Time 80 minutes, obtaining outward appearance is grayish powder, surveys particle diameter, D90=4.33 μm, D50==1.98 μm;
8, the material after step 7 ball milling is dried, packed.
Embodiment 3
Waste and old high-cerium rare-earth polishing powder after the present embodiment uses with optical manufacturing factory polishing departement is for raw material, and concrete steps are as follows:
1, make waste and old polishing powder from rare earth and water in mass ratio 1:4 mix and soak, soak 1.8 hours;
2, the mixed solution in step 1 is filtered and 800 object fine screen mesh filtration treatment through 80 object wide-meshed screens successively, remove the impurity that particle is larger;
3, dry after the filtrate precipitation in step 2, bake out temperature 200 DEG C, realizes the purification of waste and old polishing powder from rare earth;
4, the waste and old polishing powder after step 3 purification is carried out to the mensuration of content of rare earth and cerium-oxide contents, cerium-oxide contents is 65.10%;
5, the waste and old polishing powder from rare earth after purification described in step 4 is taken: 800g, mix together with additive I:30g, additive II:80g, grind in corundum mortar by hand, milling time 25 minutes, wherein additive I is ammonium sulfate, level Four reagent, additive main component is silicon-dioxide, provides for Suzhou Na Fang engineering materials company limited produces;
6, the material after step 5 being ground is loaded in porcelain crucible, and material brim height is the 2/3-3/4 of porcelain crucible height, recessed in the middle part of material, put into the roasting of retort furnace mouth, continuous warming to 900 DEG C, soaking time power-off after 3 hours, takes out after making material naturally cool to room temperature with stove;
7, being milled to particle diameter to material is 2.0 μm;
8, the material after step 9 ball milling is dried, packed.
Embodiment 4
Waste and old high-cerium rare-earth polishing powder after the present embodiment uses with optical manufacturing factory polishing departement is for raw material, and concrete steps are as follows:
1, make waste and old polishing powder from rare earth and water in mass ratio 1:4 mix and soak, soak 1.8 hours;
2, the mixed solution in step 1 is filtered and 1000 object fine screen mesh filtration treatment through 100 object wide-meshed screens successively, remove the impurity that particle is larger;
3, dry after the filtrate precipitation in step 2, bake out temperature 200 DEG C, realizes the purification of waste and old polishing powder from rare earth;
4, the waste and old polishing powder after step 3 purification is carried out to the mensuration of content of rare earth and cerium-oxide contents;
5, take the waste and old polishing powder from rare earth after purification described in step 4: 10kg, mix, in grinding machine for grinding together with additive I:0.4kg, additive II:1.2kg, milling time 15 minutes, wherein additive I is ammonium sulfate, level Four reagent, and additive II is silicon-dioxide;
6, the material after step 5 being ground is loaded in four large quartzy tanks, and material brim height is the 2/3-3/4 of tank body height, recessed in the middle part of material, put into the roasting of retort furnace mouth, continuous warming to 900 DEG C, soaking time power-off after 3 hours, makes material naturally cool to less than 200 DEG C with stove;
7, survey particle diameter to step 6 material, wherein survey particle diameter: D90=6.7 μm, D50=3.92 μm, subsequently to material ball milling, size controlling is 2.0 μm;
8, the material after step 7 ball milling is carried out 200 DEG C of oven dry, packed.
Claims (6)
1. a waste and old polishing powder from rare earth reclaiming preparation method, is characterized in that, comprise the following steps:
Step one: the purification of waste and old polishing powder from rare earth
Waste and old polishing powder from rare earth is soaked by 1.1, soak time 1.5-2.5 hour;
1.2 to sieve process to the filtrate in step 1.1 with screen cloth, liquid precipitate post-drying to be filtered, and bake out temperature 180-220 DEG C, obtains the waste and old polishing powder from rare earth of purification;
Step 2: the selection of additive
2.1 prepare additive I: be ammonium sulfate;
2.2 prepare additive II: be silicon-dioxide;
Step 3: waste and old polishing powder from rare earth is with the proportioning of additive
Waste and old polishing powder from rare earth after purification mixes by following mass ratio with additive by 3.1: the discarded polishing powder from rare earth after purification: 100 parts, additive I:1-5 part, additive II:5-15 part;
3.2 by mixed for step 3.1 material grinding 5-30 minute;
Step 4: the roasting regeneration of waste and old polishing powder from rare earth
4.1 step 3.2 is ground after material tinning and carry out roasting, wherein maturing temperature 700-1000 DEG C, roasting time 2-6 hour;
After 4.2 power-off, allow material naturally cool to after below 300 DEG C and material is taken out;
Material after 4.3 pairs of step 4.2 roastings carries out ball milling, is milled to desired particle size;
Material after step 4.3 ball milling carries out drying, packing by 4.4.
2. the reclaiming preparation method of a kind of waste and old polishing powder from rare earth according to claim 1, is characterized in that: in described step 1.1, the mass ratio of water and waste and old polishing powder from rare earth is 4:1.
3. the reclaiming preparation method of a kind of waste and old polishing powder from rare earth according to claim 1, is characterized in that: select the screen cloth of 50-100 order and 500-1000 object to sieve process to the mixed solution in step 1.1 in described step 1.2 successively.
4. the reclaiming preparation method of a kind of waste and old polishing powder from rare earth according to claim 1, is characterized in that: mixed by following mass ratio with additive by the waste and old polishing powder from rare earth after purification in described step 3.1: the discarded polishing powder from rare earth after purification: 100 parts, additive I:4 part, additive II:10 part.
5. the reclaiming preparation method of a kind of waste and old polishing powder from rare earth according to claim 1, is characterized in that: can add appropriate pure zirconia cerium powder in described step 3.1 as required.
6. the reclaiming preparation method of a kind of waste and old polishing powder from rare earth according to claim 1, is characterized in that: in described step 4.1, maturing temperature is 900 DEG C, roasting time 4 hours.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113214791A (en) * | 2021-04-30 | 2021-08-06 | 惠晶显示科技(苏州)有限公司 | Method for extracting grinding powder from etching waste and recycling grinding powder |
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CN102167956A (en) * | 2011-03-07 | 2011-08-31 | 长沙翰林化工科技有限公司 | Method for recycling and reutilizing rare-earth polishing powder waste residue and waste liquor |
CN102357398A (en) * | 2011-06-17 | 2012-02-22 | 金华冠华水晶有限公司 | Method for separating each component in waste residue in crystal industry |
JP2013086204A (en) * | 2011-10-17 | 2013-05-13 | Shinryo Corp | Method for reproducing cerium oxide-based abrasive slurry and reproduced cerium oxide-based abrasive slurry |
CN103215012A (en) * | 2013-04-26 | 2013-07-24 | 济南大学 | Preparation method for regenerating rear-earth polishing powder |
CN103965791A (en) * | 2014-05-07 | 2014-08-06 | 连云港健发磁性材料有限公司 | Clean rapid regeneration method of waste rare-earth polishing powder |
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- 2015-07-23 CN CN201510437815.0A patent/CN104962200A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102167956A (en) * | 2011-03-07 | 2011-08-31 | 长沙翰林化工科技有限公司 | Method for recycling and reutilizing rare-earth polishing powder waste residue and waste liquor |
CN102357398A (en) * | 2011-06-17 | 2012-02-22 | 金华冠华水晶有限公司 | Method for separating each component in waste residue in crystal industry |
JP2013086204A (en) * | 2011-10-17 | 2013-05-13 | Shinryo Corp | Method for reproducing cerium oxide-based abrasive slurry and reproduced cerium oxide-based abrasive slurry |
CN103215012A (en) * | 2013-04-26 | 2013-07-24 | 济南大学 | Preparation method for regenerating rear-earth polishing powder |
CN103965791A (en) * | 2014-05-07 | 2014-08-06 | 连云港健发磁性材料有限公司 | Clean rapid regeneration method of waste rare-earth polishing powder |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113214791A (en) * | 2021-04-30 | 2021-08-06 | 惠晶显示科技(苏州)有限公司 | Method for extracting grinding powder from etching waste and recycling grinding powder |
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Application publication date: 20151007 |