The preparation method of the adulterated zirconium white composite polishing of a kind of cerium powder
Technical field
The present invention relates to the polishing powder from rare earth technical field of material, the preparation method of the adulterated zirconium white composite polishing of particularly a kind of cerium powder.
Background technology
Cerium oxide is widely used in polishings such as opticglass, lens, liquid crystal display, semi-conductor as the best rare-earth polishing material of effect, and what be only second to its polishing effect is zirconium white, but zirconic work-ing life is poor than cerium oxide.
Because rare earth is a kind of strategic goods and materials; at present; country has put into effect rare earth protectiveness policy; not only to the strict control of rare earth exploitation having carried out; and significantly raised the rare earth export quotas, protected the rare earth resources of China's preciousness not to be wasted, therefore; with the rare earths material is the preparation and the application of the polishing material of matrix, is subjected to the restriction and the high restriction of price of raw material sources.Simultaneously, existing is in the preparation process of polishing material of matrix, to need to use materials such as hydrofluoric acid, silicofluoric acid, fluorinated, acid ammonium with the rare earths material, and these materials have bigger harm to environment and human body.
Summary of the invention
At the existing in prior technology deficiency, technical problem to be solved by this invention provides and a kind ofly is matrix, can substitutes polishing powder from rare earth and feature of environmental protection polishing material preparation method preferably in preparation process with non-rare earths material.
The technical solution used in the present invention is the preparation method of the adulterated zirconium white composite polishing of a kind of cerium of invention powder, and its technical process is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 150g/L-200g/L, become zirconium salt solution, standby;
B, get a certain amount of cerium salt, join in the standby zirconium salt solution, become zirconates cerium mixed salt solution by the 5%-7% of zirconates amount, standby;
C, get a certain amount of organic bases, being mixed with organic bases content is the organic bases solution of 200g/L-300g/L, and adds the organic solvent that occupies machine alkaline solution gross weight 0.05%-0.5%, mixes, and becomes alkaline solution, standby;
D, with above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stirring, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 2-1: 6, and temperature of reaction is controlled at 40-100 ℃; After treating that neutralization reaction fully, extraordinarily go into oxygenant according to the 2-5 of cerium zirconium mass ratio, and stop to stir ageing 2-6 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, must zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing was carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, zirconium cerium mixture, standby;
G, with standby zirconium cerium mixture through 850-1300 ℃ of temperature calcining 2-4 hour, promptly get the adulterated zirconium white composite polishing of cerium powder;
H, described zirconates are a kind of in hydration zirconium oxychloride, hydration zirconium carbonate, the nitric hydrate oxygen zirconium; Described cerium salt is a kind of in nitric hydrate cerium, the hydration Cerium II Chloride; Described organic bases is a kind of in ammoniacal liquor, urea, the vulkacit H or two kinds or three kinds; Described oxygenant is that a kind of in hydrogen peroxide, potassium permanganate, the potassium perchlorate or two kinds or three kinds are as oxygenant; Described organic solvent is polyoxyethylene glycol, polyacrylic acid, organosilyl a kind of or two kinds or three kinds.
The technical process of the technical scheme of its optimization is as follows:
A, get certain amount of zirconium salt, be mixed with the aqueous solution that zirconates content is 180g/L-190g/L, become zirconium salt solution, standby;
B, get a certain amount of cerium salt, join in the standby zirconium salt solution, become zirconates cerium mixed salt solution by the 5%-7% of zirconates amount, standby;
C, get a certain amount of organic bases, being mixed with organic bases content is the organic bases solution of 250g/L-260g/L, and adds the organic solvent that occupies machine alkaline solution gross weight 0.1%-0.2%, mixes, and becomes alkaline solution, standby;
D, with above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, wherein the mol ratio of the active substance of zirconates cerium mixed salt solution and alkaline solution is 1: 3-1: 5; Temperature of reaction is controlled at 50-80 ℃; After treating that neutralization reaction fully, extraordinarily go into oxygenant according to the 2-5 of cerium amount ratio, and stop to stir ageing 3-5 hour; Then, filter, get throw out, standby;
E, with standby throw out washing 2-4 time, must zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing was carried out freeze-day with constant temperature 24 hours under 85-150 ℃ of temperature, zirconium cerium mixture, standby;
G, with standby zirconium cerium mixture through 900-1100 ℃ of temperature calcining 2-4 hour, promptly get the adulterated zirconium white composite polishing of cerium powder.
In above-mentioned each technical scheme, when preparing alkaline solutions for two kinds in employing ammoniacal liquor, urea, the vulkacit H or three kinds, the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
In adopting hydrogen peroxide, potassium permanganate, potassium perchlorate two kinds or three kinds are as oxygenant, and the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
When adopting poly(oxyethylene glycol) 400, polyacrylic acid, organosilyl two kinds or three kinds of preparation organic solvents, the general mol ratio equivalent of required alkaline solution that adopts of the consumption of its each component is prepared;
The preparation method of the adulterated zirconium white composite polishing of cerium of the present invention powder, the employing zirconium white is a matrix, a spot of cerium oxide that mixes, by the neutralization of organic bases, the gained throw out becomes through high-temperature calcination, thereby, saved a large amount of rare earth materials; Simultaneously, in preparation process, do not need to use the material such as hydrofluoric acid, silicofluoric acid, fluorinated, acid ammonium that environment and human body is had bigger harm, so its feature of environmental protection is better.Its product " the adulterated zirconium white composite polishing of cerium powder " through overtesting, has polishing effect preferably, below is cerium adulterated zirconium white composite polishing powder and polishing powder from rare earth polishing effect contrast table:
The sample title |
The smooth finish grade |
Scratch the bar number |
Surface adhesive |
Cerium doped zirconia composite polishing powder |
High |
Few |
A little less than |
Polishing powder from rare earth |
Low |
Many |
By force |
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.Following explanation is to adopt the mode that exemplifies, but protection scope of the present invention should not be limited to this.
Embodiment one:
The preparation method of the adulterated zirconium white composite polishing of the cerium of present embodiment powder, its technical process is as follows: A, get 1308g hydration zirconium oxychloride, join in the 7L water, preparation becomes zirconium salt solution, and is standby;
B, get 55g hydration Cerium II Chloride, join in the standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, and is standby;
C, get 589g ammoniacal liquor, be dissolved in the 2.3L water, and add the 4.6g poly(oxyethylene glycol) 400, mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After treating that neutralization reaction fully, add the 10g hydrogen peroxide, and stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing was carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, zirconium cerium mixture, standby;
G, with standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, promptly get 525 and restrain the adulterated zirconium white composite polishing of ceriums powder.
Embodiment two:
The preparation method of the adulterated zirconium white composite polishing of the cerium of present embodiment powder, its technical process is as follows:
A, get 1190g hydration zirconium carbonate, join in the 6.6L water, preparation becomes zirconium salt solution, and is standby;
B, get 45g nitric hydrate cerium, join in the standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, and is standby;
C, get 568g ammoniacal liquor and 11g urea, be dissolved in the 2.3L water, and add the 4.6g poly(oxyethylene glycol) 400, mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After treating that neutralization reaction fully, add 5g hydrogen peroxide, 45g potassium permanganate, and stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing was carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, zirconium cerium mixture, standby;
G, with standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, promptly get 525 and restrain the adulterated zirconium white composite polishing of ceriums powder.
Embodiment three:
The preparation method of the adulterated zirconium white composite polishing of the cerium of present embodiment powder, its technical process is as follows:
A, get 1742g nitric hydrate oxygen zirconium, join in the 9.6L water, preparation becomes zirconium salt solution, and is standby;
B, get 45g nitric hydrate cerium, join in the standby zirconium salt solution, preparation becomes zirconates cerium mixed salt solution, and is standby;
C, get 497g ammoniacal liquor, 37g urea, 81g vulkacit H, be dissolved in the 2.5L water, and add the 5.0g polyacrylic acid, mix, become alkaline solution, standby;
D, with above-mentioned standby zirconates cerium mixed salt solution under the condition of heating, slowly add above-mentioned standby alkaline solution while stir, carry out neutralization reaction, temperature of reaction is controlled at 50 ℃; After treating that neutralization reaction fully, add 3.8g hydrogen peroxide, 30.6g potassium permanganate, 26.8g potassium perchlorate, and stop to stir ageing 4 hours; Then, filter, get throw out, standby;
E, with standby throw out washing 3 times, zirconium cerium composite precipitation thing, standby;
F, standby zirconium cerium composite precipitation thing was carried out freeze-day with constant temperature 24 hours under 95 ℃ of temperature, zirconium cerium mixture, standby;
G, with standby zirconium cerium mixture through 950 ℃ of temperature calcining 3 hours, promptly get 525 and restrain the adulterated zirconium white composite polishing of ceriums powder.
Use the preparation method of the adulterated zirconium white composite polishing of cerium of the present invention powder, the adulterated zirconium white composite polishing of the cerium of preparation powder can be used for polishings such as opticglass, lens, liquid crystal display, semi-conductor.