CN109897552A - A kind of preparation method of lanthanum cerium mischmetal polishing powder - Google Patents
A kind of preparation method of lanthanum cerium mischmetal polishing powder Download PDFInfo
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- CN109897552A CN109897552A CN201711399250.7A CN201711399250A CN109897552A CN 109897552 A CN109897552 A CN 109897552A CN 201711399250 A CN201711399250 A CN 201711399250A CN 109897552 A CN109897552 A CN 109897552A
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Abstract
The present invention relates to a kind of preparation methods of lanthanum cerium mischmetal polishing powder, comprising the following steps: 1. lanthanum carbonate cerium mischmetal raw material is dissolved with hydrochloric acid solution, obtains lanthanum-cerium chloride liquid；2. adjusting lanthanum-cerium chloride liquid pH value with sodium hydroxide solution；3. being fluorinated；4. ammonium carbonate tune pH value is added to 7-8, it is aged 3-4 hours, washes 3-4 times；5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；6. polishing powder from rare earth carbonate precursor crystallizes, plate compression is carried out, roasting obtains the product of uniform particle sizes.This method technological operation is simple, and low in raw material price, production cost is low, the high-performance lanthanum cerium mischmetal polishing powder for being suitble to the expeditiously prepared sizes of heavy industrialization uniform.
Description
Technical field
The present invention relates to a kind of preparation methods of polishing powder from rare earth, and in particular to a kind of even-grained lanthanum cerium mischmetal polishing
The preparation method of powder.
Background technique
With the rapid development of electronics and information industry at home and abroad, the application field of polishing powder from rare earth is also constantly changing,
Polished by traditional TV display tube glass bulb, water drilling polishing etc. to liquid crystal display, compared with precision optical instrument device contour
It can the transformation of polishing powder field；In terms of development trend, field of liquid crystal display and high-grade optical manufacturing field are that polishing powder from rare earth adds deeply
The application development direction of work.High-grade polishing powder from rare earth is widely used in plate glass, cathode-ray tube, teleputer and shows
The polishing of the devices such as device, glass bulb, spectacle lens, optical glass, camera lens, jewel, crystal, ornament.The lanthanum cerium of even particle size distribution
Polishing powder from rare earth added value is high, and profit is big, and closely related with the high and new technology field of high speed development, and application prospect is long-range.
Currently, being corresponded at present for different raw materials different there are many kinds of the raw materials of China's production polishing powder from rare earth
Preparation process such as utilizes high-purity cerium dioxide (CeO2> 99%) it is raw material, through high-temperature roasting, water quenching, classification, filtering, drying etc.
Process prepares high cerium polishing powder；Using fluoro-carbon-cerium ore concentrate as raw material, using solid reaction process, through processes systems such as crushing, roasting, classifications
Standby cerium polishing powder low out；With mixed rare earth carbonate (CeO2Account for 45% or so) it is raw material, it is fired production rare earth oxide, then
CeO (OH) is obtained with acid processing2Precipitating and trivalent rare earth solution wash CeO (OH)2CeO is obtained after precipitating, dry, roasting2Contain
The high cerium polishing powder etc. in 98%-99% is measured, there are many disadvantages for these: first is that the rare earth component fluctuation of mine is larger, to cause
Cerium content in product is unstable, and product quality also fluctuates therewith；Second is that containing the radioactive elements such as thorium and uranium, radiation in mine
Property element can be brought into product in this process, bring in production and in pollution；Third is that non-rare earth impurity content in mine
It crosses high.
Patent CN101899281B discloses a kind of polishing powder from rare earth and preparation method thereof, the polishing powder contain cerium oxide,
Lanthana, praseodymium oxide, total amount of rare earth TREO cerium-oxide contents in 90wt% or more, polishing powder from rare earth total amount of rare earth TREO
Ratio account for 70-80%, the ratio 19-29% of lanthanum oxide content, praseodymium oxide content ratio accounts for 0.05-2%；Although joined fluorine
F element needs more to control preliminarily forming for product granularity, but as the production such as plate glass, camera lens need high-precision to polish
Add the polishing powder of uniform particle size, to obtain the good lapped face of polishing effect.
Summary of the invention
Drawbacks described above can be overcome the present invention provides one kind, prepared using common lanthanum carbonate cerium as raw material, by fluorination and
Ultrasonic wave homogenize process prepares precursor, finally to realize the controllable preparation side of lanthanum cerium mischmetal polishing Powder Particle Size
Method, this method technological operation is simple, and low in raw material price, production cost is low, is suitble to expeditiously preparing for heavy industrialization
The high-performance lanthanum cerium mischmetal polishing powder of homogeneous grain diameter.
Technical solution of the present invention:
A kind of preparation method of lanthanum cerium mischmetal polishing powder, comprising the following steps:
1. lanthanum carbonate cerium mischmetal raw material is dissolved with hydrochloric acid solution, lanthanum-cerium chloride liquid, rare-earth oxidation in lanthanum-cerium chloride liquid are obtained
Object total amount is 300-350g/L；
2. adjusting lanthanum-cerium chloride liquid pH value to 4-4.5 with sodium hydroxide solution；
3. being fluorinated, hydrofluoric acid is added after fluorination, the mass ratio that control F accounts for total amount of rare earth is 1-1.5%；
4. ammonium carbonate tune pH value is added to 7-8, it is aged 3-4 hours, washes 3-4 times, matter in lanthanum carbonate cerium is controlled after washing
It measures content Cl and is less than 0.12wt%, Ba is less than 0.02wt%, and Ca is less than 0.35wt%；
5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；
6. polishing powder from rare earth carbonate precursor crystallizes 3-5h, plate compression is carried out, roasting obtains the product of uniform particle sizes.
Further, step 1. in lanthanum carbonate cerium mischmetal ingredient requirement: the accounting of total amount of the rare earth oxide is greater than 40wt%,
Cerium oxide CeO2Content is 65wt%-70wt% in the ratio of total amount of the rare earth oxide, and the concentration of the hydrochloric acid solution is 1mol/
L。
Further, step 2. in sodium hydrate aqueous solution concentration be 6mol/L.
Further, step 3. in fluorinated materials HF content be greater than 20wt%, ignition residue is less than 0.001wt%, clearly
Clear transparent no tobacco.
Further, step 4. in ammonium carbonate in impurity B a, Pb, Al content be respectively less than 0.01wt%, do not agglomerate loosely,
White not burnt hair, the pollution-free no moisture absorption.
Further, step 5. middle ultrasonic wave homogenizing processing are as follows: every 1h, unlatching ultrasonic wave circular treatment is primary, single
Handle time 10min-30min；The power regulating range of ultrasonic wave: 1000-3000W, ultrasonic frequency adjustable range: 10KHz-
The unlatching of 40KHz, circulating pump start simultaneously with the unlatching of ultrasonic wave, accumulate sonication treatment time 2-3h.
Further, 6. middle crystallization temperature is 28-30 DEG C, crystallization time 2.5-3h, calcining time 2.5-3h to step, roasting
Burn 800-1000 DEG C of temperature.
The present invention obtains the product index of uniform particle sizes: D50 is 1.6-2.6 μm, and total amount of rare earth TREO is 45wt%-
50wt%, wherein cerium oxide accounts for the 65%-70% of total amount of the rare earth oxide, and colours white band is light red.
Beneficial effects of the present invention:
The method of the present invention simple process, production cost is low, with short production cycle, high production efficiency；This method successfully solves rare earth
The polishing disadvantage that Powder Particle Size is uneven, impurity is high, the polishing powder Granularity Distribution section of preparation is small, and homogeneity is good, enriches me
State's polishing powder product specification reduces domestic down-stream enterprise to the dependence of international high-end polishing powder product, to promote the country more
The common progress and development of a industry.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1
A kind of preparation method of lanthanum cerium mischmetal polishing powder, comprising the following steps:
1. lanthanum carbonate cerium mischmetal raw material is dissolved with hydrochloric acid solution, lanthanum-cerium chloride liquid, rare-earth oxidation in lanthanum-cerium chloride liquid are obtained
Object total amount is 300g/L；
2. adjusting lanthanum-cerium chloride liquid pH value to 4-4.5 with sodium hydroxide solution；
3. being fluorinated, hydrofluoric acid is added after fluorination, the mass ratio that control F accounts for total amount of rare earth is 1-1.5%；
4. ammonium carbonate tune pH value is added to 7, it is aged 3 hours, washes 3 times, mass content in lanthanum carbonate cerium is controlled after washing
Cl is less than 0.12wt%, and Ba is less than 0.02wt%, and Ca is less than 0.35wt%；
5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；
6. polishing powder from rare earth carbonate precursor crystallizes 3h, plate compression is carried out, roasting obtains the product of uniform particle sizes.
Further, step 1. in lanthanum carbonate cerium mischmetal ingredient requirement: the accounting of total amount of the rare earth oxide is greater than 40wt%,
Cerium oxide CeO2Content is 65wt% in the ratio of total amount of the rare earth oxide, and the concentration of the hydrochloric acid solution is 1mol/L.
Further, step 2. in sodium hydrate aqueous solution concentration be 6mol/L.
Further, step 3. in fluorinated materials HF content be greater than 20wt%, ignition residue is less than 0.001wt%, clearly
Clear transparent no tobacco.
Further, step 4. in ammonium carbonate in impurity B a, Pb, Al content be respectively less than 0.01wt%, do not agglomerate loosely,
White not burnt hair, the pollution-free no moisture absorption.
Further, step 5. middle ultrasonic wave homogenizing processing are as follows: every 1h, unlatching ultrasonic wave circular treatment is primary, single
Handle time 10min；The power regulating range of ultrasonic wave: 1000W, ultrasonic frequency adjustable range: 10KHzKHz, circulating pump
Unlatching starts simultaneously with the unlatching of ultrasonic wave, accumulates sonication treatment time 2h.
Further, 6. middle crystallization temperature is 28 DEG C, crystallization time 2.5h, calcining time 2.5h to step, maturing temperature
800℃。
Obtained product index: D50 is 2.0 μm, and total amount of rare earth TREO is 48wt%, and wherein cerium oxide accounts for rare earth oxide
The 65% of total amount, colours white band are light red.
Embodiment 2
A kind of preparation method of lanthanum cerium mischmetal polishing powder, comprising the following steps:
1. lanthanum carbonate cerium mischmetal raw material is dissolved with hydrochloric acid solution, lanthanum-cerium chloride liquid, rare-earth oxidation in lanthanum-cerium chloride liquid are obtained
Object total amount is 350g/L；
2. adjusting lanthanum-cerium chloride liquid pH value to 4.5 with sodium hydroxide solution；
3. being fluorinated, hydrofluoric acid is added after fluorination, the mass ratio that control F accounts for total amount of rare earth is 1.5%；
4. ammonium carbonate tune pH value is added to 8, it is aged 4 hours, washes 4 times, mass content in lanthanum carbonate cerium is controlled after washing
Cl is less than 0.12wt%, and Ba is less than 0.02wt%, and Ca is less than 0.35wt%；
5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；
6. polishing powder from rare earth carbonate precursor crystallizes 5h, plate compression is carried out, roasting obtains the product of uniform particle sizes.
Further, step 1. in lanthanum carbonate cerium mischmetal ingredient requirement: the accounting of total amount of the rare earth oxide is greater than 40wt%,
Cerium oxide Ce02 content is 70wt% in the ratio of total amount of the rare earth oxide, and the concentration of the hydrochloric acid solution is 1mol/L.
Further, step 2. in sodium hydrate aqueous solution concentration be 6mol/L.
Further, step 3. in fluorinated materials HF content be greater than 20wt%, ignition residue is less than 0.001wt%, clearly
Clear transparent no tobacco.
Further, step 4. in ammonium carbonate in impurity B a, Pb, Al content be respectively less than 0.01wt%, do not agglomerate loosely,
White not burnt hair, the pollution-free no moisture absorption.
Further, step 5. middle ultrasonic wave homogenizing processing are as follows: every 1h, unlatching ultrasonic wave circular treatment is primary, single
Handle time 30min；The power regulating range of ultrasonic wave: 3000W, ultrasonic frequency adjustable range: 40KHz, circulating pump are opened
It opens the unlatching with ultrasonic wave and starts simultaneously, accumulate sonication treatment time 3h.
Further, 6. middle crystallization temperature is 30 DEG C, crystallization time 3h, calcining time 3h to step, maturing temperature 1000
℃。
The present invention obtains the product index of uniform particle sizes: D50 is 1.8 μm, total amount of rare earth TREO is 50wt%, wherein oxygen
Change cerium and account for the 69% of total amount of the rare earth oxide, colours white band is light red.
Embodiment 3
A kind of preparation method of lanthanum cerium mischmetal polishing powder, comprising the following steps:
1. lanthanum carbonate cerium mischmetal raw material is dissolved with hydrochloric acid solution, lanthanum-cerium chloride liquid, rare-earth oxidation in lanthanum-cerium chloride liquid are obtained
Object total amount is 320g/L；
2. adjusting lanthanum-cerium chloride liquid pH value to 4 with sodium hydroxide solution；
3. being fluorinated, hydrofluoric acid is added after fluorination, the mass ratio that control F accounts for total amount of rare earth is 1.2%；
4. ammonium carbonate tune pH value is added to 7.5, it is aged 3.5 hours, washes 3 times, quality in lanthanum carbonate cerium is controlled after washing
Content C1 is less than 0.12wt%, and Ba is less than 0.02wt%, and Ca is less than 0.35wt%；
5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；
6. polishing powder from rare earth carbonate precursor crystallizes 4h, plate compression is carried out, roasting obtains the product of uniform particle sizes.
Further, step 1. in lanthanum carbonate cerium mischmetal ingredient requirement: the accounting of total amount of the rare earth oxide is greater than 40wt%,
Cerium oxide CeO2Content is 68wt% in the ratio of total amount of the rare earth oxide, and the concentration of the hydrochloric acid solution is 1mol/L.
Further, step 2. in sodium hydrate aqueous solution concentration be 6mol/L.
Further, step 3. in fluorinated materials HF content be greater than 20wt%, ignition residue is less than 0.001wt%, clearly
Clear transparent no tobacco.
Further, step 4. in ammonium carbonate in impurity B a, Pb, Al content be respectively less than 0.01wt%, do not agglomerate loosely,
White not burnt hair, the pollution-free no moisture absorption.
Further, step 5. middle ultrasonic wave homogenizing processing are as follows: every 1h, unlatching ultrasonic wave circular treatment is primary, single
Handle time 20min；The power regulating range of ultrasonic wave: 2000W, ultrasonic frequency adjustable range: 20KHz, circulating pump are opened
It opens the unlatching with ultrasonic wave and starts simultaneously, accumulate sonication treatment time 2.5h.
Further, 6. middle crystallization temperature is 29 DEG C, crystallization time 2.5h, calcining time 3h to step, maturing temperature 900
℃。
The present invention obtains the product index of uniform particle sizes: D50 is 1.6 μm, and total amount of rare earth TREO is 45wt%, wherein aoxidizing
Cerium accounts for the 65% of total amount of the rare earth oxide, and colours white band is light red.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments in the case where not departing from the spirit or scope of the invention patent.Therefore, originally
Invention is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein
Consistent widest scope.
Claims (7)
1. a kind of preparation method of lanthanum cerium mischmetal polishing powder, which comprises the following steps: 1. lanthanum carbonate cerium mischmetal raw material
It is dissolved with hydrochloric acid solution, obtains lanthanum-cerium chloride liquid, lanthanum-cerium chloride liquid middle rare earth total amount is 300-350g/L；
2. adjusting lanthanum-cerium chloride liquid pH value to 4-4.5 with sodium hydroxide solution；
3. being fluorinated, hydrofluoric acid is added after fluorination, the mass ratio that control F accounts for total amount of rare earth is 1-1.5%；
4. ammonium carbonate tune pH value is added to 7-8, it is aged 3-4 hours, washes 3-4 times, matter in lanthanum carbonate cerium is controlled after washing
It measures content C1 and is less than 0.12wt%, Ba is less than 0.02wt%, and Ca is less than 0.35wt%；
5. carrying out the homogenize process of ultrasonic wave, the polishing powder from rare earth carbonate precursor of even particle size distribution is obtained；
6. polishing powder from rare earth carbonate precursor crystallizes 3-5h, plate compression is carried out, roasting obtains the product of uniform particle sizes.
2. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step 1. in carbonic acid
Lanthanum cerium mischmetal ingredient requirement: the accounting of total amount of the rare earth oxide is greater than 40wt%, cerium oxide CeO2Content is total in rare earth oxide
The ratio of amount is 65wt%-70wt%, and the concentration of the hydrochloric acid solution is 1mol/L.
3. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step 2. in hydrogen-oxygen
The concentration for changing sodium water solution is 6mol/L.
4. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step 3. middle fluorination
HF content is greater than 20wt% in raw material, and ignition residue is less than 0.001wt%, as clear as crystal no tobacco.
5. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step 4. in carbon
Impurity B a, Pb, Al content are respectively less than 0.01wt% in sour ammonium, do not agglomerate loosely, white not burnt hair, the pollution-free no moisture absorption.
6. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step is 5. middle ultrasonic
Wave homogenizing processing are as follows: every 1h, unlatching ultrasonic wave circular treatment is primary, single treatment time 10min-30min；The function of ultrasonic wave
Rate adjustable range: 1000-3000W, ultrasonic frequency adjustable range: 10KHz-40KHz, unlatching the opening with ultrasonic wave of circulating pump
It opens and starts simultaneously, accumulate sonication treatment time 2-3h.
7. a kind of preparation method of lanthanum cerium mischmetal polishing powder according to claim 1, which is characterized in that step 6. middle crystallization
Temperature is 28-30 DEG C, crystallization time 2.5-3h, calcining time 2.5-3h, 800-1000 DEG C of maturing temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778972A (en) * | 2021-03-10 | 2021-05-11 | 安徽禾臣新材料有限公司 | Polishing powder for fine polishing of electronic display screen and production method thereof |
| CN113651352A (en) * | 2021-09-02 | 2021-11-16 | 甘肃稀土新材料股份有限公司 | Method for preparing low-calcium cerium lanthanum carbonate from high-calcium cerium lanthanum chloride solution |
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| CN102978399A (en) * | 2012-12-12 | 2013-03-20 | 南昌大学 | Method for producing low chloride fine particle high purity rare earth compound through ultrasonic-assisted oxalate deposition |
| CN103131385A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
| CN104497887A (en) * | 2014-12-23 | 2015-04-08 | 包头市华辰稀土材料有限公司 | Method for preparing composite oxide polishing powder |
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| CN101899281A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Rare earth polishing powder and production method thereof |
| CN103131385A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
| CN102978399A (en) * | 2012-12-12 | 2013-03-20 | 南昌大学 | Method for producing low chloride fine particle high purity rare earth compound through ultrasonic-assisted oxalate deposition |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112778972A (en) * | 2021-03-10 | 2021-05-11 | 安徽禾臣新材料有限公司 | Polishing powder for fine polishing of electronic display screen and production method thereof |
| CN113651352A (en) * | 2021-09-02 | 2021-11-16 | 甘肃稀土新材料股份有限公司 | Method for preparing low-calcium cerium lanthanum carbonate from high-calcium cerium lanthanum chloride solution |
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