CN101215446A - Method for preparing high-cerium nano-stage rare earth polishing powder from rare earth ore concentrate - Google Patents
Method for preparing high-cerium nano-stage rare earth polishing powder from rare earth ore concentrate Download PDFInfo
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- CN101215446A CN101215446A CNA2007100001127A CN200710000112A CN101215446A CN 101215446 A CN101215446 A CN 101215446A CN A2007100001127 A CNA2007100001127 A CN A2007100001127A CN 200710000112 A CN200710000112 A CN 200710000112A CN 101215446 A CN101215446 A CN 101215446A
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Abstract
A method for preparing rare-earth polish powder in high cerium nanometer magnitude from rare earth ore concentrate, which is characterized in that the producing steps comprise directly preparing mixed carbonic acid rare-earth from rare earth ore concentrate dense sulphating roasting and infusion with a method of precipitating ammonium acid carbonate, mixing the mixed carbonic acid rare-earth and alkali 0.5-2 parts, heating to 600-800 DEG C to melt the compound, keeping the temperature for 1-4 hours in the molten state, cooling, grinding, then, adding industrial hydrofluoric acid HF>=45% whose adding amount is 10%-20% of the weight of rare-earth concentrate powder, and obtaining oxyfluoride rare earth enriched products, the oxyfluoride rare earth enriched products are grinded, watered, water filtered, mixed in a mixer, then packed into a high-energy ball mill with sieve, and filled with nitrogen, wet powder is ball-abraded with high energy, a high pressure current rotary passage is arranged on the lower portion of a rear sieve of a high-energy ball mill room, the water of sieved powder is dried under the impetus of high speed currents and then baked, and finished polish powder whose powder particle size is <=500nm is obtained.
Description
Technical field
The present invention relates to a kind of production method of utilizing rare earth ore concentrate to produce high-cerium nano magnitude polishing powder from rare earth.
Background technology
In military and defence engineering, many weaponrys need precise polished.Polishing powder from rare earth is adopted in this polishing mostly.The production of polishing powder from rare earth, the technology that domestic and international most producers adopt are to be intermediates such as rare earth hydrate, carbonated rare earth with feedstock conversion such as rare earth oxide, sulfuric acid rare earths, it are fluoridized again, and roasting then, grinding, sorting make finished product.This explained hereafter nano level powder size polishing powder, technology is numerous and diverse, the cost height, the finished powder recovery rate is low, is unfavorable for the widespread use of the polishing powder from rare earth of nano-scale powder.Also having a kind of is to decompose rare earth ore concentrate and directly make the production technique of rare earth hydrate intermediate with hot alkaline solution, and this explained hereafter time is long, can not prepare≤powder of 1 μ m powder size, is unfavorable for large-scale production.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of production method of utilizing rare earth ore concentrate to produce high-cerium nano magnitude polishing powder from rare earth.The polishing powder production cost that this production method is produced is low, and the cycle is short, and the powder degree can carry out precise polished to the weaponry and the product for civilian use below 50-500nm.
For this reason, technical scheme of the present invention is: a kind of rare earth ore concentrate prepares the method for high-cerium nano magnitude polishing powder from rare earth, it is characterized in that: production stage is for directly to make mixed rare earth carbonate with ammonium bicarbonate precipitation method from rare earth ore concentrate concentrated sulfuric acid roasting, infusion; Mixed rare earth carbonate mixes with 0.5-2 part alkali, be heated to 600-800 ℃, make the mixture fusion, and in molten state insulation 1-4 hour, cool off, pulverize, add then the industrial hydrofluoric acid of HF 〉=45%, its add-on is the 10%-20% of rare earth ore concentrate grain weight amount, obtains fluorine rare earth oxide enriched substance; The rare enriched substance of fluorine oxidation is pulverized, washing, and drainage, even in stirrer for mixing, pack into then in the band sieve high energy ball mill, charge into nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel, and undersized powder dries processing to the moisture of powder under high velocity air promotes, dry again, powder size≤500nm to the finished product polishing powder.
The production method of described rare earth sodium rice polishing powder is characterized in that: rare earth ore concentrate powder, RE
2O
3, its grade is 40%-80%; Ammonium bicarbonate precipitation method directly makes mixed rare earth carbonate from rare earth ore concentrate concentrated sulfuric acid roasting infusion, evenly the water wet-milling adds the high-energy ball milling of protecting gas and the high speed rotating air-flow flouring technology to the drying of powder.
The present invention is owing to adopt the rare earth ore concentrate powder, and this is that the production technique of raw material is compared in adopting rare earth chloride, can significantly reduce production cost of products; Adopt ammonium bicarbonate precipitation and vitriol oil roast, water logging to decompose rare earth ore concentrate in the production process of the present invention, it is fast that this method has decomposition rate, the characteristics of complete decomposition; Thereafter even water wet-milling adds the high-energy ball milling of protecting gas and high speed rotating air-flow makes nano-scale powder non-agglomerate and whole production process cycle short to the flouring technology of the drying of powder.
Embodiment
Ammonium bicarbonate precipitation method be rare earth ore concentrate in concentrated sulfuric acid roasting, water logging and the infusion after the removal of impurities, add the ammonium bicarbonate precipitation agent, the reactional equation of rare earth and bicarbonate of ammonia is as follows:
RE2(SO4)3+6NH4HCO3+xH2O→RE2
(CO3)3·xH2O↓+3(NH4)2SO4+3CO2↑+3H2O
Excessive bicarbonate of ammonia can generate the carbonated rare earth double salt precipitation with rare earth:
8NH4HCO3+RE2(SO4)3+yH2O→RE2
(CO3)3·(NH4)2CO3·yH2O↓+3(NH4)2SO4+4CO2+4H2O
Owing to exist a large amount of SO2-4 and NH4+ may have the reaction of formation rare earth sulfuric acid double salt to take place in the system:
2RE3++2NH+4+4SO2-4+8H2O→RE2(SO4)3·(NH4)2SO4·8H2O↓
The solubility with temperature of rare earth sulfuric acid double salt raises and descends.Infusion directly mixes with solid ammonium bicarbonate, does not add tensio-active agent or flocculation agent, and precipitation promptly gets carbonated rare earth through ageing, washing, vacuum filtration or whizzer drying;
The purpose of washing is to remove residual alkali and solubility salt.Make the pH value of carbonated rare earth enriched substance reach 7-8.But the washing proceed step by step, promptly first cold water embathes, and can embathe several times, to pH value near 8, boil at hot water and to wash, to PH near 7.
The industrial hydrofluoric acid that contains HF 〉=45% is adopted in fluoridizing of carbonated rare earth enriched substance, and its add-on is the 10%-20% of rare earth ore concentrate grain weight amount, obtains fluorine rare earth hydrate RE (OH) 2F enriched substance.
The present invention adopts and is with the air-flow high-energy ball milling, plays the powder grinding on the one hand, works to break up poly-group of powder and drying on the other hand.Said air-flow is the nitrogen of circulating pressure 1-2MPa.
Novel process is than other polishing powder from rare earth production technique, 2000 yuan of cost decreases per ton, and the rare earth yield improves more than 11%; The polishing powder from rare earth powder that novel process is produced is tiny, has improved the grade of polishing powder from rare earth.It is big that this polishing powder has specific surface area, long service life, good, the easy cleaning of polishing smooth finish, suspension well, characteristics such as non-environmental-pollution, can be used for the grinding and polishing of high precision such as opticglass, picture tube glass bulb, ic substrate glass, electroplating substrate glass, aircraft toughened glass, silicon single crystal flake, various display glass.
Embodiment 1
Rare earth ore concentrate powder and bicarbonate of ammonia add the fusion vitriol oil again, roast under 650 ℃ of temperature, and the add-on of the vitriol oil is 30% of a rare earth ore concentrate grain weight amount, and constantly stirs, and it is fully reacted, and directly makes mixed rare earth carbonate in the infusion; Mixed rare earth carbonate mixes with 1 part of alkali, is heated to 800 ℃, makes the mixture fusion, and, cooling, pulverize, add then 45% industrial hydrofluoric acid in molten state insulation 3 hours, its add-on is 20% of a rare earth ore concentrate grain weight amount, obtain fluorine rare earth oxide enriched substance, the rare enriched substance of fluorine oxidation is pulverized, washing, drainage, even in stirrer for mixing, in the band sieve high energy ball mill of packing into then, charge into 1MPa nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel, undersized powder is under high velocity air promotes, moisture to powder dries processing, dry again, powder size≤500nm to the finished product polishing powder, gained polishing powder from rare earth index: total amount of rare earth (TREO) 92%, cerium oxide content 85%, average powder degree 0.2 μ m, pH value 6.7.
Embodiment 2
Rare earth ore concentrate powder and bicarbonate of ammonia add the fusion vitriol oil again, roast under 800 ℃ of temperature, and the add-on of the vitriol oil is 20% of a rare earth ore concentrate grain weight amount, and constantly stirs, and it is fully reacted, and directly makes mixed rare earth carbonate in the infusion; Mixed rare earth carbonate mixes with 2 parts of alkali, is heated to 700 ℃, makes the mixture fusion, and, cooling, pulverize, add then 45% industrial hydrofluoric acid in molten state insulation 2 hours, its add-on is 15% of a rare earth ore concentrate grain weight amount, obtain fluorine rare earth oxide enriched substance, the rare enriched substance of fluorine oxidation is pulverized, washing, drainage, even in stirrer for mixing, in the band sieve high energy ball mill of packing into then, charge into 1.5MPa nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel, undersized powder is under high velocity air promotes, moisture to powder dries processing, dry again, powder size≤500nm to the finished product polishing powder, gained polishing powder from rare earth index: total amount of rare earth (TREO) 92%, cerium oxide content 85%, average powder degree 0.2 μ m, pH value 6.7.
Gained polishing powder from rare earth index: total amount of rare earth (TREO) 93%, cerium oxide content 85%, average powder degree 0.25 μ m, pH value 7.2.
The above; it only is better embodiment of the present invention; should not be regarded as limitation of the scope of the invention; and the claim scope that the present invention advocated is not limited thereto; all personages who is familiar with this field skill; according to the disclosed technology contents of the present invention, can think easily and equivalence change, all should fall within the scope of protection of the present invention.
Claims (2)
1. a rare earth ore concentrate prepares the method for high-cerium nano magnitude polishing powder from rare earth, and it is characterized in that: production stage is for directly to make mixed rare earth carbonate with ammonium bicarbonate precipitation method from rare earth ore concentrate concentrated sulfuric acid roasting, infusion; Mixed rare earth carbonate mixes with 0.5-2 part alkali, be heated to 600-800 ℃, make the mixture fusion, and be incubated 14 hours in molten state, cool off, pulverize, add then the industrial hydrofluoric acid of HF 〉=45%, its add-on is the 10%-20% of rare earth ore concentrate grain weight amount, obtains fluorine rare earth oxide enriched substance; The rare enriched substance of fluorine oxidation is pulverized, washing, and drainage, even in stirrer for mixing, pack into then in the band sieve high energy ball mill, charge into nitrogen, carry out the wet-milling high-energy ball milling; The below of sieving behind the high-energy ball milling chamber has the high pressure draft rotating channel, and undersized powder dries processing to the moisture of powder under high velocity air promotes, dry again, powder size≤500nm to the finished product polishing powder.
2. the described rare earth ore concentrate of claim 1 prepares the method for high-cerium nano magnitude polishing powder from rare earth, it is characterized in that: rare earth ore concentrate powder, RE
2O
3, its grade is 40%-80%; Ammonium bicarbonate precipitation method directly makes mixed rare earth carbonate from rare earth ore concentrate concentrated sulfuric acid roasting infusion, evenly the water wet-milling adds the high-energy ball milling of protecting gas and the high speed rotating air-flow flouring technology to the drying of powder.
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| CNA2007100001127A CN101215446A (en) | 2007-01-05 | 2007-01-05 | Method for preparing high-cerium nano-stage rare earth polishing powder from rare earth ore concentrate |
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| CNA2007100001127A CN101215446A (en) | 2007-01-05 | 2007-01-05 | Method for preparing high-cerium nano-stage rare earth polishing powder from rare earth ore concentrate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671525B (en) * | 2009-09-01 | 2013-04-10 | 湖南皓志新材料股份有限公司 | Method for improving suspension property of rare earth polishing powder |
| CN104673098A (en) * | 2013-11-28 | 2015-06-03 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
-
2007
- 2007-01-05 CN CNA2007100001127A patent/CN101215446A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671525B (en) * | 2009-09-01 | 2013-04-10 | 湖南皓志新材料股份有限公司 | Method for improving suspension property of rare earth polishing powder |
| CN104673098A (en) * | 2013-11-28 | 2015-06-03 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
| CN104673098B (en) * | 2013-11-28 | 2017-01-18 | 安阳工学院 | Preparation technique of cerium-oxide-base rare-earth polishing powder |
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Open date: 20080709 |