CN101037217A - Production method of ultra granule yttria - Google Patents
Production method of ultra granule yttria Download PDFInfo
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- CN101037217A CN101037217A CN 200710027240 CN200710027240A CN101037217A CN 101037217 A CN101037217 A CN 101037217A CN 200710027240 CN200710027240 CN 200710027240 CN 200710027240 A CN200710027240 A CN 200710027240A CN 101037217 A CN101037217 A CN 101037217A
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Abstract
The present invention provides a preparation method of superfine yttrium oxide. The yttrium oxide solution and oxalic acid solution are subjected to homogeneous precipitation in a co-precipitation manner with an error of 4~6% and a reaction time of 10~20 minutes; wherein the yttrium oxide solution has a concentration of 40~100 g/l, a pH value of 2 and a temperature of 15~25 DEG C; the oxalic acid solution has a concentration of 8~10% and a temperature of 15~25 DEG C. Then, polybutanol serving as dispersant is added into the homogeneous precipitation solution, wherein the dosage of polybutano is 0.1~0.3% by volume of the total amount of the precipitation solution, and the obtained precipitation solution is filtered for 10~20 minutes to separate the mother liquor and the precipitate, then the precipitate is scrubbed for 3~5 times, filtered, and roasted at 850~900 DEG C for 3~3.5 hours, thereby, the superfine yttrium oxide (D50 less than 1 um)is obtained. The present invention has the advantages of simple manufacturing technique, high product quality, excellent size distribution, uniform particle displayed under ultramicroscope, smooth and shining surface, no hardened layer, excellent physical property; besides, when the superfine yttrium oxide is used for fluorescent powder, the light colour is good, the light wane and the color temperature are excellent.
Description
Technical field
The invention belongs to field of new, relate to a kind of production method of ultra granule yttria.
Background technology
Rerum naturas such as yttria particles particle diameter directly have influence on the quality and the purposes of derived product, and ultra granule yttria shows extremely people's concern of excellent properties because of it in fields such as light, electricity, physical-chemical reactions.Produce ultra-fine grain medium particle diameter D at present
50The method of=0.1～1 μ m yttrium oxide mainly contains physics method and chemical method.The physics method mainly contains: 1, physical pulverization method, by the blast of mechanical disintegration, electrical spark, the ultrasonic wave ultra granule yttria that obtains such as cracked, be characterized in simple to operate, cost is low, but product purity is low, and size distribution is inhomogeneous, surface irregularity, particularly after fragmentation, crystal grain rerum natura deterioration and cause performance index to descend.2, mechanical wet ball mill method is adding the macrobead yttrium oxide under the water condition, and the ball milling yttrium oxide through dehydration, oven dry, roasting, be characterized in simple to operate, but product purity is low, and size distribution is inhomogeneous, and operation is loaded down with trivial details, to equipment requirements height, investment greatly.Chemical method mainly contains: 1, microemulsion method, two kinds of immiscible solvents form milk sap under the effect of tensio-active agent, in microvesicle, form nuclear, coalescent, reunion, thermal treatment and obtain ultra-fine grain particle, the monodispersity and the interface property that are characterized in particle are good, size distribution is even, but its solvent cost height, complex process, wayward.2, the precipitator method are controlled certain condition, precipitation agent is joined in the yttrium solution reaction after, sedimentation and filtration, calcination are obtained ultra granule yttria, be characterized in simple, production cost is low, and equipment requirements is low, drop into for a short time, but particle diameter is bigger and wayward, and size distribution is undesirable.
Summary of the invention
It is easy that purpose of the present invention just provides a kind of production technique, and size distribution and particle rerum natura are good, the production method of the ultra granule yttria that product performance are good.
The technical solution adopted in the present invention is: with yttrium chloride solution and oxalic acid solution precipitation from homogeneous solution (PFHS), add dispersion agent in the precipitation, throw out separates mother liquor after filtration, wash 3-5 time, vacuum filtration, calcination then after, obtain ultra-fine grain D
50＜1 μ m yttrium oxide.
Yttrium chloride solution concentration 40～100g/L, pH value 2,15～25 ℃ of temperature; Oxalic acid solution concentration 8～10%, 15～25 ℃ of temperature, oxalic acid adding weight are 2～2.2 times of precipitating rare earth weight; When yttrium chloride solution and oxalic acid solution precipitation from homogeneous solution (PFHS), precipitate with heavy mode with polarization, be that yttrium chloride solution and oxalic acid solution are when reinforced synchronously, 4～6% of yttrium chloride solution volume joins in the precipitation vessel prior to oxalic acid solution, and yttrium chloride solution added in advance than oxalic acid solution in 1～2 minute, sedimentation time 10～20 minutes after oxalic acid solution adds, continues to stir 1～2 minute; Dispersion agent is poly-butanols, and the add-on of poly-butanols is 1 of yttrium chloride solution volume～3 ‰; Sedimentation and filtration separates 10～20 minutes mother liquor time; 850～900 ℃ of calcination temperatures, calcination time 3～3.5 hours.
Production technique of the present invention is easy, the quality product height, and size distribution is good, shows uniform particles under ultramicroscope, the slick and sly light in surface, no hardened layer, the particle rerum natura is good, is applied to fluorescent material and can improves luminosity, and photochromic good, and light decay, colour temperature are good.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment one
Getting the 1000L yttrium chloride solution transfers concentration to be 40g/L, to transfer 15 ℃ of pH value 2, temperature with pure ammoniacal liquor with pure water; Get the 80Kg high-purity oxalic acid, be mixed with concentration 8% oxalic acid solution 1000L, 15 ℃ of temperature; The yttrium chloride solution that with 4% volume is 40L earlier joins in the precipitin reaction pot, start the precipitin reaction pot and stir, add the poly-butanol solution of 1L, poly-butanols can effectively suppress the growth of crystal grain and the absorption of reuniting, precipitation system is become evenly, and product is not introduced impurity and influenced performance; Yttrium chloride solution added in advance than oxalic acid solution in 1 minute, sedimentation time 10 minutes, calculating yttrium chloride solution adding speed is 50.53L/min, concentration 8% oxalic acid solution adding speed is 100L/min, join simultaneously in the precipitin reaction pot by pump, valve and spinner-type flowmeter control yttrium chloride solution and oxalic acid solution adding speed with calculated amount, after oxalic acid solution has added, continue to stir 1 minute, total sedimentation time is 11 minutes, and polarization precipitates improving the size distribution situation and reducing the coprecipitated effect of having clear improvement of non-rare earth impurity with heavy mode; Put down being precipitated to the vacuum suction filter groove and filtering out mother liquor, 10 minutes time, separate mother liquor within a short period of time reducing a precipitation material and grow up and the impurity absorption effect that has clear improvement; Then, in the suction strainer groove, fill it up with pure water and wash 3 times, last vacuum suction filter, obtain yttrium oxalate 153.5kg, yttrium oxalate was contained in the combustion type roller kiln under 850 ℃ of temperature calcination 3 hours with healthy and free from worry alms bowl, obtained 39.3kg yttrium oxide product, product yield 98.25%.
Detect by analysis: total amount of rare earth 99.35%, igloss 0.62%, chlorine root 100ppm, granularity D
50=0.88 μ m.
Embodiment two
Getting the 500L yttrium chloride solution transfers concentration to be 100g/L, to transfer 25 ℃ of pH value 2, temperature with pure ammoniacal liquor with pure water; Get the 110kg high-purity oxalic acid, be mixed with concentration 10% oxalic acid solution 1100L, 25 ℃ of temperature; The yttrium chloride solution that with 6% volume is 30L earlier joins in the precipitation tank in term, starts precipitation tank in term and stirs, and adds the poly-butanol solution of 1.5L; Yttrium chloride solution added in advance than oxalic acid solution in 2 minutes, sedimentation time 20 minutes, calculating yttrium chloride solution adding speed is 26.11L/min, concentration 10% oxalic acid solution adding speed is 55L/min, join in the precipitation tank in term by pump, valve and spinner-type flowmeter control yttrium chloride solution and oxalic acid solution simultaneously with the adding speed of calculated amount, after oxalic acid solution adds, continue to stir 2 minutes, total sedimentation time is 22 minutes; Put down and be precipitated to the vacuum suction filter groove and filter out mother liquor, 20 minutes time; Filling it up with pure water then in the suction strainer groove washes 5 times, last vacuum suction filter obtains yttrium oxalate 199.25Kg, and yttrium oxalate is contained in the interior calcination 3.5 hours under 900 ℃ of temperature of combustion type roller kiln with healthy and free from worry alms bowl, obtain 49.01Kg yttrium oxide product, product yield 98.02%.
Detect by analysis: total amount of rare earth 99.48%, igloss 0.47%, chlorine root 40ppm, granularity D
50=0.94 μ m.
The present invention has the advantages that production technology is simple, production cost is low, properties of product are good.
Claims (8)
1, a kind of production method of ultra granule yttria is characterized in that yttrium chloride solution and oxalic acid solution precipitation from homogeneous solution (PFHS), adds dispersion agent in the precipitation, and throw out separates mother liquor after filtration, after wash water 3～5 times, vacuum filtration, the calcination, obtains ultra-fine grain D
50＜1 μ m yttrium oxide.
2, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that yttrium chloride solution concentration 40～100g/L, pH value 2,15～25 ℃ of temperature.
3, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that oxalic acid solution concentration 8～10%, and 15～25 ℃ of temperature, oxalic acid adding weight are 2～2.2 times of precipitating rare earth weight.
4, the production method of a kind of ultra granule yttria according to claim 1, when it is characterized in that yttrium chloride solution and oxalic acid solution precipitation from homogeneous solution (PFHS), precipitate with heavy mode with polarization, be that yttrium chloride solution and oxalic acid solution are when reinforced synchronously, 4～6% of yttrium chloride solution volume joins in the precipitation vessel prior to oxalic acid solution, and yttrium chloride solution added in advance than oxalic acid solution in 1～2 minute.
5, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that sedimentation time 10～20 minutes.
6, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that dispersion agent is poly-butanols, and its add-on is 1 of yttrium chloride solution volume～3 ‰.
7, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that sedimentation and filtration separates 10～20 minutes mother liquor time.
8, the production method of a kind of ultra granule yttria according to claim 1 is characterized in that 850～900 ℃ of calcination temperatures, calcination time 3～3.5 hours.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475333B (en) * | 2008-11-25 | 2011-07-20 | 当阳市公路管理段 | Asphalt antistripping agent |
| CN102139908A (en) * | 2011-04-21 | 2011-08-03 | 赣州虔东稀土集团股份有限公司 | Submicron yttrium oxide and preparation method thereof |
| CN102167973A (en) * | 2011-03-07 | 2011-08-31 | 福建省长汀金龙稀土有限公司 | Preparation method of 3-5 micron yttrium-europium oxide |
| 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 |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
| CN106044832A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of yttrium oxide with central grain size being 20-50 microns |
| CN107099681A (en) * | 2017-05-16 | 2017-08-29 | 广东富远稀土新材料股份有限公司 | A kind of method of extract and separate yttrium |
| CN108408754A (en) * | 2018-02-05 | 2018-08-17 | 常州市卓群纳米新材料有限公司 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
-
2007
- 2007-03-22 CN CN 200710027240 patent/CN101037217A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475333B (en) * | 2008-11-25 | 2011-07-20 | 当阳市公路管理段 | Asphalt antistripping agent |
| CN102167973A (en) * | 2011-03-07 | 2011-08-31 | 福建省长汀金龙稀土有限公司 | Preparation method of 3-5 micron yttrium-europium oxide |
| CN102167973B (en) * | 2011-03-07 | 2013-08-21 | 福建省长汀金龙稀土有限公司 | Preparation method of 3-5 micron yttrium-europium oxide |
| CN102139908A (en) * | 2011-04-21 | 2011-08-03 | 赣州虔东稀土集团股份有限公司 | Submicron yttrium oxide and preparation method thereof |
| CN102139908B (en) * | 2011-04-21 | 2012-09-12 | 赣州虔东稀土集团股份有限公司 | Submicron yttrium oxide 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 |
| CN103803630A (en) * | 2014-01-27 | 2014-05-21 | 福建省长汀金龙稀土有限公司 | Method for preparing yttria of different sizes and different appearances |
| CN106044832A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of yttrium oxide with central grain size being 20-50 microns |
| CN107099681A (en) * | 2017-05-16 | 2017-08-29 | 广东富远稀土新材料股份有限公司 | A kind of method of extract and separate yttrium |
| CN107099681B (en) * | 2017-05-16 | 2018-07-10 | 广东富远稀土新材料股份有限公司 | A kind of method of extraction and separation yttrium |
| CN108408754A (en) * | 2018-02-05 | 2018-08-17 | 常州市卓群纳米新材料有限公司 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
| CN108408754B (en) * | 2018-02-05 | 2019-11-12 | 常州市卓群纳米新材料有限公司 | A kind of resistant to plasma being conducive to color after control sprays corrodes the preparation method of granulation yttrium oxide used for hot spraying |
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Open date: 20070919 |