CN104017500A - Preparation method of rare earth polishing powder - Google Patents
Preparation method of rare earth polishing powder Download PDFInfo
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- CN104017500A CN104017500A CN201410256001.2A CN201410256001A CN104017500A CN 104017500 A CN104017500 A CN 104017500A CN 201410256001 A CN201410256001 A CN 201410256001A CN 104017500 A CN104017500 A CN 104017500A
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Abstract
The invention discloses a preparation method of rare earth polishing powder. The preparation method comprises the following steps of (1) precipitating mixed rare earth through an ammonium hydrogen carbonate and ammonia water mixed solution, ageing, and then, adding mixed fluorine-contained acid to fluorinate to obtain fluorinated alkaline rare earth carbonate, wherein mixed rare earth is cerium lanthanum chloride rare earth or cerium lanthanum chloride rare earth, and mixed fluorine-contained acid is mixed acid of hydrofluoric acid and fluosilicic acid; (2) carrying out multi-stage roasting on fluorinated alkaline rare earth carbonate obtained in the step (1) to obtain a mixed rare earth oxide, wherein the mixed rare earth oxide is an oxygen cerium fluoride and cerium oxide mixture or an oxygen cerium lanthanum fluoride and cerium oxide mixture; (3) smashing the mixed rare earth oxide obtained in the step (2), and grading to obtain the rare earth polishing powder with the particle size of 0.3-0.5mu m. The preparation method can be used for preparing ultrafine rare earth polishing powder which is capable of reaching the angstrom grade on a glass polished surface, uniform in dispersion and small in particle size.
Description
Technical field
The present invention relates to a kind of preparation method of polishing powder from rare earth.
Background technology
The general tradition of polishing powder from rare earth is for the polishing of lens, sheet glass, glass bulb, glasses, watchcase etc., in recent years, at aspects such as function ceramics, catalysis, luminous, gas sensor, fuel cell and ultraviolet radiation absorption, is widely used.In addition, more and more higher to the function of polishing powder from rare earth and performance requriements, particularly finish size and the surface requirements of blue glass are more and more higher at present, the granularity of existing polishing powder and the gap of polishing performance are larger, rare earth polishing has been invented by some producer, by chemical action, improve polishing powder and polishing environment solves, yet correspondingly brought environmental issue.At present, polishing powder from rare earth is generally made by bakes to burn the article, and temperature is higher, and the polishing powder burning is out harder, can not meet the demands.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of polishing powder from rare earth, can prepare the superfine rare earth polishing powder to glass polishing surface reaches dust level, is uniformly dispersed, particle diameter is little.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, the mixing solutions by bicarbonate of ammonia and ammoniacal liquor precipitates, after ageing, add mixing fluoric-containing acid to fluoridize, the basic carbonate rare earth that obtains fluoridizing, wherein, mishmetal is lanthanum-cerium chloride rare earth or lanthanum-cerium chloride praseodymium rare earth, and mixing fluoric-containing acid is the mixing acid of hydrofluoric acid, silicofluoric acid;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained carries out multistage roasting, obtains mixed rare-earth oxide, and wherein, mixed rare-earth oxide is the mixture of oxygen cerium fluoride and cerium oxide, or the mixture of oxygen lanthanum fluoride cerium and cerium oxide;
(3) mixed rare-earth oxide obtaining in step 2 is carried out to crushing and classification, obtain polishing powder from rare earth, its grain graininess is 0.3 ~ 0.5 μ m.
Preferably, in lanthanum-cerium chloride rare earth of the present invention, the massfraction of cerium oxide is 75 ~ 90%, and the massfraction of lanthanum trioxide is 10 ~ 25%; In described lanthanum-cerium chloride praseodymium rare earth, the massfraction of cerium oxide is 73 ~ 88%, and the massfraction of lanthanum trioxide is 10 ~ 25%, and the massfraction of Praseodymium trioxide is 0.5 ~ 3%.
Preferably, in the mixing solutions of bicarbonate of ammonia of the present invention and ammoniacal liquor, the mass ratio of bicarbonate of ammonia, ammoniacal liquor is 1:1 ~ 2.
Preferably, in mixing fluoric-containing acid of the present invention, the mass ratio of hydrofluoric acid, silicofluoric acid is 4 ~ 6:1, and the mass ratio that mixes fluoric-containing acid and mishmetal is 5 ~ 7%.
Preferably, in step 1 of the present invention, temperature during precipitation is 45 ~ 55 ℃, and the time of ageing is 12 ~ 18 hours.
Preferably, in step 2 of the present invention, the step of multistage roasting is as follows:
First paragraph was warming up to 420 ~ 510 ℃ in 1 ~ 1.5 hour;
Second segment is incubated roasting 6 ~ 10 hours at 420 ~ 510 ℃;
The 3rd section: in 4 ~ 5 hours, from holding temperature, be warming up to 840 ~ 920 ℃.
The 4th section: at 840 ~ 920 ℃, be incubated 9 ~ 15 hours.
Preferably, in step 2 of the present invention, multistage roasting is carried out in shuttle-type industrial furnace.
Preferably, in step 3 of the present invention, crushing and classification carries out in accurate air classification pulverizer, and during crushing and classification, the rotating speed of the impeller of pulverizer is 130 ~ 139Hz, and air pressure is 0.9Mpa.
Therefore compared with prior art, the present invention has following beneficial effect:
1, by mixing ammonia solution, make basic carbonate rare earth, possessed the character of carbonated rare earth and rare earth hydrate, roasting changes polishing powder at low temperatures, has reduced the energy and devices consume, has saved production cost;
2, with hydrofluoric acid and silicofluoric acid, carry out fluoridation, obtain fluorine-containing polishing powder, by multistage roasting, fluorine-containing basic carbonate rare earth is easily obtained the better oxygen cerium fluoride of polishing powder performance or oxygen lanthanum fluoride cerium again, the polishing powder that contains these two kinds of materials can reach dust () level to glazed surface;
3, in stage reduction process, by improving the gap of classifying turbine sheet and the rotating speed that weight improves impeller, the ultra-fine polishing powder that makes to produce is uniformly dispersed, particle diameter is less.
Embodiment
Below in conjunction with specific embodiment, describe the present invention in detail, in this illustrative examples of the present invention and explanation, be used for explaining the present invention, but not as a limitation of the invention.
Embodiment mono-
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 75%, the massfraction of lanthanum trioxide is 25%) mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor is 1:1) precipitation by bicarbonate of ammonia and ammoniacal liquor under temperature 45 C, ageing 12 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 7%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 420 ℃ for 1.5 hours;
Second segment is incubated roasting 8 hours at 420 ℃;
The 3rd section: within 4 hours, from 460 ℃, be warming up to 920 ℃;
The 4th section: at 920 ℃, be incubated 12 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 139Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment bis-
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 80%, the massfraction of lanthanum trioxide is 20%) at 55 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 18 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 7%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 440 ℃ for 1.5 hours;
Second segment is incubated roasting 8 hours at 460 ℃;
The 3rd section: within 4 hours, from 460 ℃, be warming up to 880 ℃;
The 4th section: at 880 ℃, be incubated 12 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 139Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment tri-
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 75%, the massfraction of lanthanum trioxide is 25%) mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor is 1:2) precipitation by bicarbonate of ammonia and ammoniacal liquor under temperature 50 C, ageing 12 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 5:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 6%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 480 ℃ for 1.5 hours;
Second segment is incubated roasting 12 hours at 480 ℃;
The 3rd section: within 4 hours, from 480 ℃, be warming up to 900 ℃;
The 4th section: at 900 ℃, be incubated 15 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 130Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment tetra-
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 78%, the massfraction of lanthanum trioxide is 20%, the parts by weight of Praseodymium trioxide are 2%) at 52 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 12 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 5:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 6%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 460 ℃ for 1.5 hours;
Second segment is incubated roasting 8 hours at 460 ℃;
The 3rd section: within 4 hours, from 460 ℃, be warming up to 920 ℃;
The 4th section: at 920 ℃, be incubated 12 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 132Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment five
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 77%, the massfraction of lanthanum trioxide is 20%, the parts by weight of Praseodymium trioxide are 3%) at 54 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 18 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 7%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 450 ℃ for 1.5 hours;
Second segment is incubated roasting 9 hours at 450 ℃;
The 3rd section: within 4 hours, from 450 ℃, be warming up to 900 ℃.
The 4th section: at 900 ℃, be incubated 10 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 135Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment six
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 79%, the massfraction of lanthanum trioxide is 19%, the parts by weight of Praseodymium trioxide are 2%) at 48 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 16 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 6:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 5%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 440 ℃ for 1.5 hours;
Second segment is incubated roasting 9 hours at 440 ℃;
The 3rd section: within 4 hours, from 440 ℃, be warming up to 890 ℃.
The 4th section: at 890 ℃, be incubated 12 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 133Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment seven
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 80%, the massfraction of lanthanum trioxide is 20%) at 46 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1.5) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 13 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4.5:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 5.5%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 450 ℃ for 1.1 hours;
Second segment is incubated roasting 7 hours at 450 ℃;
The 3rd section: within 4.2 hours, from 450 ℃, be warming up to 850 ℃;
The 4th section: at 850 ℃, be incubated 10 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 139Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment eight
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 85%, the massfraction of lanthanum trioxide is 15%) at 47 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1.6) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 14 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 5.5:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 6.5%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 470 ℃ for 1.2 hours;
Second segment is incubated roasting 6 hours at 470 ℃;
The 3rd section: within 4.4 hours, from 470 ℃, be warming up to 860 ℃;
The 4th section: at 860 ℃, be incubated 11 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 139Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment nine
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 73%, the massfraction of lanthanum trioxide is 25%, the parts by weight of Praseodymium trioxide are 2%) at 48 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 15 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4.2:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 5.6%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 500 ℃ for 1.4 hours;
Second segment is incubated roasting 6.5 hours at 500 ℃;
The 3rd section: within 4.6 hours, from 500 ℃, be warming up to 910 ℃.
The 4th section: at 910 ℃, be incubated 14 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 133Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment ten
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 88%, the massfraction of lanthanum trioxide is 10%, the parts by weight of Praseodymium trioxide are 2%) at 51 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1.8) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 17 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 4.8:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 6.4%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 440 ℃ for 1.5 hours;
Second segment is incubated roasting 9 hours at 440 ℃;
The 3rd section: within 4 hours, from 440 ℃, be warming up to 890 ℃.
The 4th section: at 890 ℃, be incubated 12 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 133Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment 11
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 86%, the massfraction of lanthanum trioxide is 13.5%, the parts by weight of Praseodymium trioxide are 0.5%) at 53 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1.4) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 17 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 6.8:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 5.6%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 470 ℃ for 1.2 hours;
Second segment is incubated roasting 7.5 hours at 470 ℃;
The 3rd section: within 4.8 hours, from 470 ℃, be warming up to 855 ℃;
The 4th section: at 855 ℃, be incubated 12.5 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 133Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
Embodiment 12
The preparation method of polishing powder from rare earth, comprises the following steps:
(1) by mishmetal, (massfraction of cerium oxide is 85%, the massfraction of lanthanum trioxide is 15%, the parts by weight of Praseodymium trioxide are 3%) at 49 ℃ of temperature by mixing solutions (mass ratio of bicarbonate of ammonia, ammoniacal liquor the is 1:1.9) precipitation of bicarbonate of ammonia and ammoniacal liquor, ageing 17.5 hours, then (mass ratio of hydrofluoric acid, silicofluoric acid is 5.2:1 to add mixing fluoric-containing acid, the mass ratio that mixes fluoric-containing acid and mishmetal is 6.6%) fluoridize the basic carbonate rare earth that obtains fluoridizing;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained is put into shuttle-type industrial furnace and is carried out roasting, obtains mixed rare-earth oxide, and calcination steps is as follows:
First paragraph, is warming up to 490 ℃ for 1.1 hours;
Second segment is incubated roasting 8.5 hours at 490 ℃;
The 3rd section: within 4.9 hours, from 490 ℃, be warming up to 865 ℃.
The 4th section: at 865 ℃, be incubated 9.5 hours;
(3) will in the accurate air classification pulverizer of the mixed rare-earth oxide obtaining in step 2, carry out crushing and classification, the rotating speed of the impeller of pulverizer is 133Hz, and air pressure is 0.9Mpa, obtains polishing powder from rare earth, and its grain graininess is 0.3 ~ 0.5 μ m.
The technical scheme above embodiment of the present invention being provided is described in detail, applied specific case herein the principle of the embodiment of the present invention and embodiment are set forth, the explanation of above embodiment is only applicable to help to understand the principle of the embodiment of the present invention; , for one of ordinary skill in the art, according to the embodiment of the present invention, in embodiment and range of application, all will change, in sum, this description should not be construed as limitation of the present invention meanwhile.
Claims (8)
1. a preparation method for polishing powder from rare earth, is characterized in that: comprise the following steps:
(1) by mishmetal, the mixing solutions by bicarbonate of ammonia and ammoniacal liquor precipitates, after ageing, add mixing fluoric-containing acid to fluoridize, the basic carbonate rare earth that obtains fluoridizing, wherein, mishmetal is lanthanum-cerium chloride rare earth or lanthanum-cerium chloride praseodymium rare earth, and mixing fluoric-containing acid is the mixing acid of hydrofluoric acid, silicofluoric acid;
(2) the basic carbonate rare earth of fluoridizing step 1 being obtained carries out multistage roasting, obtains mixed rare-earth oxide, and wherein, mixed rare-earth oxide is the mixture of oxygen cerium fluoride and cerium oxide, or the mixture of oxygen lanthanum fluoride cerium and cerium oxide;
(3) mixed rare-earth oxide obtaining in step 2 is carried out to crushing and classification, obtain polishing powder from rare earth, its grain graininess is 0.3 ~ 0.5 μ m.
2. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described lanthanum-cerium chloride rare earth, the massfraction of cerium oxide is 75 ~ 90%, and the massfraction of lanthanum trioxide is 10 ~ 25%; In described lanthanum-cerium chloride praseodymium rare earth, the massfraction of cerium oxide is 73 ~ 88%, and the massfraction of lanthanum trioxide is 10 ~ 25%, and the massfraction of Praseodymium trioxide is 0.5 ~ 3%.
3. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in the mixing solutions of described bicarbonate of ammonia and ammoniacal liquor, the mass ratio of bicarbonate of ammonia, ammoniacal liquor is 1:1 ~ 2.
4. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described mixing fluoric-containing acid, the mass ratio of hydrofluoric acid, silicofluoric acid is 4 ~ 6:1, and the mass ratio that mixes fluoric-containing acid and mishmetal is 5 ~ 7%.
5. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described step 1, temperature during precipitation is 45 ~ 55 ℃, and the time of ageing is 12 ~ 18 hours.
6. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described step 2, the step of multistage roasting is as follows:
First paragraph was warming up to 420 ~ 510 ℃ in 1 ~ 1.5 hour;
Second segment is incubated roasting 6 ~ 10 hours at 420 ~ 510 ℃;
The 3rd section: in 4 ~ 5 hours, from holding temperature, be warming up to 840 ~ 920 ℃;
The 4th section: at 840 ~ 920 ℃, be incubated 9 ~ 15 hours.
7. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described step 2, multistage roasting is carried out in shuttle-type industrial furnace.
8. the preparation method of polishing powder from rare earth according to claim 1, is characterized in that: in described step 3, crushing and classification carries out in accurate air classification pulverizer, and during crushing and classification, the rotating speed of the impeller of pulverizer is 130 ~ 139Hz, and air pressure is 0.9Mpa.
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| CN104371554A (en) * | 2014-10-17 | 2015-02-25 | 乐山东承新材料有限公司 | Lanthanum cerium fluoride oxide rare earth polishing liquid |
| CN104774561A (en) * | 2015-03-27 | 2015-07-15 | 南昌大学 | Method for preparing rare earth polishing powder and recovering ammonium salt by using fluorine-containing niobium-tantalum wastewater |
| CN105038604A (en) * | 2015-06-01 | 2015-11-11 | 华东理工大学 | Composition and preparation method of fluorine-containing rare-earth composite oxides |
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| CN108659714A (en) * | 2018-05-11 | 2018-10-16 | 内蒙古包钢和发稀土有限公司 | The production method of Rare earth oxide polishing powder raw material |
| CN110872471A (en) * | 2018-08-30 | 2020-03-10 | 惠州比亚迪实业有限公司 | Cerium oxide polishing solution and preparation method and application thereof |
| CN112358185A (en) * | 2020-11-30 | 2021-02-12 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel base coat and preparation method thereof |
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| CN104371554B (en) * | 2014-10-17 | 2017-07-11 | 乐山东承新材料有限公司 | Fluorine cerium lanthanum oxide rare earth polishing |
| CN104371554A (en) * | 2014-10-17 | 2015-02-25 | 乐山东承新材料有限公司 | Lanthanum cerium fluoride oxide rare earth polishing liquid |
| CN104774561A (en) * | 2015-03-27 | 2015-07-15 | 南昌大学 | Method for preparing rare earth polishing powder and recovering ammonium salt by using fluorine-containing niobium-tantalum wastewater |
| CN104774561B (en) * | 2015-03-27 | 2017-07-28 | 南昌大学 | Polishing powder from rare earth and the method for reclaiming ammonium salt are prepared using niobium tantalum fluoride waste |
| CN105038604A (en) * | 2015-06-01 | 2015-11-11 | 华东理工大学 | Composition and preparation method of fluorine-containing rare-earth composite oxides |
| CN106479374A (en) * | 2016-10-28 | 2017-03-08 | 扬州翠佛堂珠宝有限公司 | A kind of jasper polishing fluid |
| CN106566419A (en) * | 2016-10-28 | 2017-04-19 | 扬州翠佛堂珠宝有限公司 | Jade polishing powder |
| CN108659714A (en) * | 2018-05-11 | 2018-10-16 | 内蒙古包钢和发稀土有限公司 | The production method of Rare earth oxide polishing powder raw material |
| CN108659714B (en) * | 2018-05-11 | 2020-11-13 | 内蒙古包钢和发稀土有限公司 | Production method of rare earth oxide polishing powder raw material |
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| CN110872471B (en) * | 2018-08-30 | 2021-10-22 | 惠州比亚迪实业有限公司 | Cerium oxide polishing solution and preparation method and application thereof |
| CN112358185A (en) * | 2020-11-30 | 2021-02-12 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel base coat and preparation method thereof |
| CN112358185B (en) * | 2020-11-30 | 2023-06-09 | 湖南景翌湘台环保高新技术开发有限公司 | Enamel primer and preparation method thereof |
| CN113817412A (en) * | 2021-11-05 | 2021-12-21 | 巴彦淖尔市亿鑫新材料有限责任公司 | Preparation method of nano polishing powder |
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