CN101381092B - Method for preparing large granularity and large specific surface area spherical yttrium oxide - Google Patents
Method for preparing large granularity and large specific surface area spherical yttrium oxide Download PDFInfo
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Abstract
The invention relates to a method for preparing spherical yttria with large granularity and large specific surface area, in particular to a method for preparing the spherical yttria with large granularity and large specific surface area by an yttric inorganic salt solution through an ammonium hydrogen carbonate precipitation method. The preparation method comprises the following steps: the yttricinorganic salt solution and the ammonium hydrogen carbonate aqueous solution directly react to generate a serous fluid containing yttrium carbonate; and subsequently, the serous fluid is added with soluble ammonium salt and is kept stand, matured, filtered, washed and calcined to manufacture the controllable spherical yttria with the granularity D50 of between 20 and 100 mu m and the specific surface area of between 10 and 100 m<2>/g. The soluble ammonium salt is added to reach the aims of regulating and controlling the size of the granularity and the specific surface area of an yttria powder body. An yttria product with large granularity and large specific surface area simultaneously is obtained by the method; sediment has large granularity; the serous fluid has good filtering performance, thereby being easy for industrialized operation; and the whole process is simple and is not limited by special equipment.
Description
Technical field
The present invention relates to the preparation method of a kind of volume particle size, large specific surface area spherical yttrium oxide, belong to preparing technical field with special rerum natura RE oxide powder material.
Technical background
Yttrium oxide powder is a kind of important high-performance ceramics raw material, is to use one of more rare earth oxide in the fluorescent material.Yttrium oxide powder has good heat-resisting, corrosion-resistant and high-temperature stability; To the reducing medium good stability; Specific inductivity high (12-14); In the application meeting in fields such as electronics, material, Aeronautics and Astronautics, nuclear power and high-performance ceramics more and more widely, therefore also can be increasingly high to the requirement of the particle size of yttrium oxide powder and specific surface area.Novel high-performance rare earth catalyst and fluorescent material all require yttrium oxide powder that big surface-area is arranged in order to improve catalytic reaction activity and luminous efficiency.The yttrium oxide powder specific surface area increases with the reduction of powder granule size, can not satisfy the requirement of macrobead bigger serface simultaneously.And when being applied to field such as spray material and resin filling materials, the pattern that often requires oxide compound is sphere or subglobular, and grain graininess is wanted big (10-60 μ m).
In order to obtain the spheric yttrium oxide powder; Spray granulation commonly used prepares spherical powder on the industrial production; Chinese patent CN1388092A disclose the globular ceramic end the preparation method, will contain the material powder raw material that ceramic constituents constitutes through nozzle and spray, thereby form drop, and make compound oxidate ceramic particle powder through the drying liq composition; Median size is 1～50 μ m, and sphericity is 0.8 or greater than 0.8.Chinese patent CN1377857 discloses a kind of working method and methods for using them of large particle ball nano ceramic powder; This method utilizes wet ball grinding to obtain the water nano colloid; Granularity is at 5-90nm; With the aqueous colloidal spraying drying, obtain the ball nano ceramic powder that macrobead is reunited, aggregated particle size is at 5-90 μ m.Chinese patent 1453243A also discloses the preparation method of large granular spherical submicron/fiber ceramics composite granule; This method obtains water base submicron/fiber ceramics colloid through wet ball grinding; Water base submicron/fiber ceramics colloid is prepared large granular spherical submicron/fiber ceramics composite granule through centrifugal or press atomization granulation; Powder median size 30-60 μ m, size distribution 10-100 μ m.But the method for spray drying method for preparation macrobead oxide compound, it is many to have operation, the shortcoming that energy consumption is big.
At present, for carbonate precipitation method that solves the problem employing that energy consumption is big and operation is many or the yttrium oxide powder that hydroxide precipitation method prepares, specific surface area can reach 30m
2/ g, but median size or median particle diameter be generally below 10 μ m, even less than 1 μ m, pattern is also mostly to be irregular pattern.Chinese patent CN1394811 and CN1394811 disclose with the salt of yttrium and alkaline solution and under tensio-active agent (or dispersion agent) existence condition, have prepared the nano level yttrium oxide, and mostly the particle that obtains is irregular polyhedron pattern.The yttrium oxide granularity that the oxalate precipitation method has preparation is bigger, and crystal formation is characteristics preferably, is often used for preparing the yttrium oxide of volume particle size, but the yttrium oxide specific surface of this method preparation is less again, less than 5m
2About/g.Chinese patent CN1629074A discloses a kind of method for preparing large particle rare-earth oxide, and this method utilizes oxalic acid to be precipitation agent, the precipitating rare earth salts solution, and like nitrate salt, with resulting drying precipitate, obtaining size-grade distribution after the calcining is normal distribution, D
50Greater than the comparatively complete hexahedron rare earth oxide of the crystal habit of 15 μ m, but there is mobile not good problem, when using, is restricted.Chinese patent CN1195647 relates to the preparation method of bigger serface, ultrafine yttria, earlier Yttrium trinitrate is dissolved in the formic acid, adds hydrazine then, the mixture of gained is calcined the yttrium oxide specific surface area that makes down in 260-360 ℃ reach 10-50m
2/ g, but granularity≤0.1 μ m.
In the wet method system, directly prepare granularity big (20-100 μ m) at present, simultaneously big (the 10-100m of specific surface area through simple softening sections of learning to do such as the precipitator method
2/ g) and for the spheric yttrium oxide does not still have report or the patent announcement.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of volume particle size, large specific surface area spherical yttrium oxide; This method is possessed volume particle size and large specific surface spheric yttrium oxide product simultaneously; The deposition granularity is big, and the dope filtration performance is good, is easy to the industriallization operation; Whole technology is simple, not limited by specific installation.
Problem to present existence; Inorganic salt solution and the ammonium bicarbonate aqueous solution direct reaction of the present invention through yttrium, the slurries of generation carbonated yttrium, again with slurries still aging after; Through filtering, wash, calcining, can obtain volume particle size (20-100 μ m), large specific surface (10-100m
2/ g) spherical yttrium oxide, and through adjustment solubility ammonium salt add-on in the slurries of carbonated yttrium, the granularity of may command ball-type yttrium oxide product.The present invention realizes through following technical scheme:
(1) adopting the inorganic salt solution of yttrium is raw material, under stirring condition, adds certain density ammonium bicarbonate soln, obtains containing the slurries of yttrium carbonate.
(2) behind reinforced the finishing, in slurries, add a certain amount of solubility ammonium salt, stir.Add the final size that the ammonium salt amount is adjusted yttrium oxide through adjustment.
(3) stop to stir, slurries are still aging at a certain temperature.In ageing process, keep sufficient standing.
(4) slurries after the ageing obtain volume particle size spherical yttrium oxide product through filtering, wash, calcining.
Among the present invention, the preferred Yttrium trinitrate of inorganic salt solution and the yttrium chloride solution of yttrium in the said step (1), concentration is 0.5-2.0mol/L.
Among the present invention, the concentration 0.5-2.0mol/L of ammonium bicarbonate soln in the said step (1).
Among the present invention, the add-on of the middle bicarbonate of ammonia of said step (1) is excellent to be the 100%-300% of theoretical add-on, the 105%-120% of preferred theoretical amount.
Among the present invention, precipitation reaction temperature is 15-40 ℃ in the said step (1), is preferably 20-30 ℃.
Among the present invention; The effect of solubility ammonium salt mainly is the ionic concn in the change system in the said step (2), makes the Zeta potential of deposit seeds take place to cause particle agglomeration property to change than about-face (seeing instance); Thereby can reach the effect of controlling final aggregation size effectively; Its basic trend is that particle surface current potential absolute value increases along with solubility ammonium salt addition increases, and an aggregation size descends and surface-area increases.Among the present invention, the solubility ammonium salt is preferably ammonium chloride, an ammonium nitrate and ammonium sulfate in the said step (2), its add-on according to concentration of slurry greater than 0 or be less than or equal to 3mol/L.
Among the present invention, still aging temperature is 15-40 ℃ described in the said step (3), is preferably 25-30 ℃; The ageing time of repose is 6-60 hour; Be preferably 12-48 hour; Of the present invention still aging be slurries in put procedure because of vibration or fluctuation do not take place in factor affecting such as external mechanical force or local heating, static ageing helps agglomerated particles all to growing up, thereby realizes the particulate nodularization.
Among the present invention, the calcining temperature described in the said step (4) is 600 ℃-1100 ℃, and it is fully decomposed, and is possessed the spherical yttrium oxide of volume particle size and bigger serface simultaneously.
The present invention has the following advantages:
1, adopt ammonium bicarbonate precipitation technology to be possessed volume particle size and large specific surface spheric yttrium oxide product simultaneously, this technology is simple, not limited by specific installation;
2, the deposition granularity is big, and the dope filtration performance is good, is easy to the industriallization operation;
3, the product granularity of gained and specific surface area can be respectively at 20-100 μ m and 10-100m
2Adjust in/g the scope.
Description of drawings
The preparation process of Fig. 1 large granular spherical yttrium oxide;
The yttrium oxide SEM photo that Fig. 2 Comparative Examples 1 prepares;
The yttrium oxide SEM photo that Fig. 3 Comparative Examples 2 prepares;
The yttrium oxide SEM photo that Fig. 4 embodiment 1 prepares;
The yttrium oxide SEM photo that Fig. 5 embodiment 5 prepares.
Among Fig. 1; The salts solution of yttrium must contain yttrium carbonate particle slurries through carbon ammonium precipitation operation 1, in slurries, adds the solubility ammonium salt, regulates the operation 2 of the surface electrical behavior of particle; Again through still aging operation 3, filter operation 4, high temperature sintering 5, obtain the large granular spherical yttrium oxide.
Embodiment
Comparative Examples 1
The characteristics of method are to contain the spraying drying operation: 50L concentration is 0.5mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins concentration 1.5mol/L down, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, after the filtration, adds Z 150PH and sizes mixing as tackiness agent, and after the employing centrifugal spray drying was handled, 720 ℃ of calcinings down can obtain the spherical yttrium oxide that granularity is 45 μ m, and specific surface area is 9.0m
2/ g, pattern are irregular spheroidal particle.
Comparative Examples 2
The characteristics of method are to contain ageing operation under whipped state: 50L concentration is 0.5mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins concentration 1.5mol/L down, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, continues to stir, and in 38 ℃ of following ageing 36h, dope filtration, washing are calcined under 720 ℃ and obtained the yttrium oxide product under whipped state, and the granularity of product is 10 μ m, and specific surface is 19.5m
2/ g, granule-morphology are the Polygons particle.
50L concentration is 0.5mol/L, and the yttrium nitrate solution of pH=4 stirs down and joins the ammonium bicarbonate soln that concentration is 0.5mol/L, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, after the bicarbonate of ammonia adding finishes, presses concentration of slurry 0.3mol/L again and adds ammonium nitrate solid; Continue to stir, after stopping to stir, still aging 36h under 38 ℃; Dope filtration, washing; Obtain the presoma powder, presoma is carried out Zeta potential measure, calcine the yttrium oxide product that obtains large granular spherical down at 720 ℃.Granularity and specific surface area to product are measured, and the result is shown in table 1.
50L concentration is 2.0mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins concentration 2.0mol/L down, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, after the bicarbonate of ammonia adding finishes, presses concentration of slurry 0.05mol/L again and adds ammonium nitrate solid; Continue to stir, after stopping to stir, still aging 36h under 38 ℃; Dope filtration, washing; Obtain the presoma powder, presoma is carried out Zeta potential measure, calcine the yttrium oxide product that obtains large granular spherical down at 720 ℃.Size ratio surface-area to product is measured, and the result is shown in table 1.
Embodiment 3
50L concentration is 1.0mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins concentration 1.0mol/L down, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, after the bicarbonate of ammonia adding finishes, presses concentration of slurry 0.10mol/L again and adds ammonium nitrate solid; Continue to stir, after stopping to stir, still aging 36h under 38 ℃; Dope filtration, washing; Obtain the presoma powder, presoma is carried out Zeta potential measure, calcine the yttrium oxide product that obtains large granular spherical down at 720 ℃.Size ratio surface-area to product is measured, and the result is shown in table 1.
50L concentration is 0.5mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins concentration 1.5mol/L down, and making the bicarbonate of ammonia consumption is 3.2 times of yttrium mole number.The deposition of adularescent generates in the bicarbonate of ammonia adition process, after the bicarbonate of ammonia adding finishes, presses concentration of slurry 0.5mol/L again and adds ammonium nitrate solid; Continue to stir, after stopping to stir, still aging 36h under 38 ℃; Dope filtration, washing; Obtain the presoma powder, presoma is carried out Zeta potential measure, calcine the yttrium oxide product that obtains large granular spherical down at 720 ℃.Size ratio surface-area to product is measured, and the result is shown in table 1.
50L concentration is 1.8mol/L, and the yttrium chloride solution of pH=3.5 stirs and joins the bicarbonate of ammonia that concentration is 0.5mol/L down; The add-on of bicarbonate of ammonia was 5.5 times of yttrium mole number, adds the chloride solid that concentration of slurry is 1.0mol/L again, in 20 ℃ of following ageings 18 hours; Filter, washing obtains the presoma powder; Presoma is carried out Zeta potential measure, obtain the yttrium oxide product in 900 ℃ of calcinings.Size ratio surface-area to product is measured, and the result is shown in table 2.
Embodiment 6
50L concentration is 1.5mol/L, and the yttrium chloride solution of pH=3.5 stirs and joins the bicarbonate of ammonia that concentration is 0.5mol/L down; The add-on that makes bicarbonate of ammonia was 5.5 times of yttrium mole number, adds the chloride solid that concentration of slurry is 2.0mol/L again, in 20 ℃ of following ageings 18 hours; Filter, washing obtains the presoma powder; Presoma is carried out Zeta potential measure, obtain the yttrium oxide product in 900 ℃ of calcinings.Size ratio surface-area to product is measured, and the result is shown in table 2.
Embodiment 7
50L concentration is 1.5mol/L, and the yttrium chloride solution of pH=3.5 stirs and joins the bicarbonate of ammonia that concentration is 0.5mol/L down; The add-on that makes bicarbonate of ammonia was 5.5 times of yttrium mole number, adds the chloride solid that concentration of slurry is 2.7mol/L again, in 20 ℃ of following ageings 18 hours; Filter, washing obtains the presoma powder; Presoma is carried out Zeta potential measure, obtain the yttrium oxide product in 900 ℃ of calcinings.Size ratio surface-area to product is measured, and the result is shown in table 2.
Embodiment 8
50L concentration is 1.0mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins 2.0mol/L down; The add-on of bicarbonate of ammonia is 4 times of yttrium mole number, and adding concentration of slurry was that 1.0mol/L ammonium sulfate and concentration of slurry are 1.0mol/L an ammonium nitrate, in 30 ℃ of following ageings 30 hours; Filter, washing obtains the presoma powder; Presoma is carried out Zeta potential measure, presoma obtains the yttrium oxide product in 900 ℃ of calcinings.The particle surface Zeta potential is the median particle D of-33 eV, product
50=34.2 μ m, specific surface area is 36.6m
2/ g.
Embodiment 9
50L concentration is 0.6mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins 2.0mol/L down; The add-on of bicarbonate of ammonia is 3 times of yttrium mole number, and adding concentration of slurry was that 1.5mol/L ammonium sulfate and concentration of slurry are 0.5mol/L an ammonium nitrate, in 40 ℃ of following ageings 6 hours; Filter; Washing, presoma obtains the yttrium oxide product in 800 ℃ of calcinings, obtains the median particle D of product
50=40.1 μ m, specific surface area is 35.0m
2The sphere of/g.
Embodiment 10
50L concentration is 0.8mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins 2.0mol/L down; The add-on of bicarbonate of ammonia is 3.5 times of yttrium mole number; Adding concentration of slurry is 3.0mol/L ammonium sulfate, in 15 ℃ of following ageings 60 hours, filters; Washing, presoma obtains the yttrium oxide product in 600 ℃ of calcinings.Obtain the median particle D of product
50=47.3 μ m, specific surface area is 31.9m
2The sphere of/g.
Embodiment 11
50L concentration is 1.1mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins 2.0mol/L down; The add-on of bicarbonate of ammonia is 5.0 times of yttrium mole number; Adding concentration of slurry is that 1.0mol/L ammonium sulfate and concentration of slurry are 0.8mol/L ammonium chloride, in 25 ℃ of following ageings 36 hours, filters; Washing, presoma obtains the yttrium oxide product in 1100 ℃ of calcinings.Obtain the median particle D of product
50=80.2 μ m, specific surface area is 28.6m
2The sphere of/g.
Embodiment 12
50L concentration is 1.3mol/L, and the yttrium nitrate solution of pH=4 stirs the ammonium bicarbonate soln that joins 2.0mol/L down; The add-on of bicarbonate of ammonia is 4.5 times of yttrium mole number; Adding concentration of slurry is that 0.8mol/L ammonium sulfate and concentration of slurry are 0.7mol/L an ammonium nitrate, in 30 ℃ of following ageings 55 hours, filters; Washing, presoma obtains the yttrium oxide product in 1000 ℃ of calcinings.The median particle D of product
50=74.4 μ m, specific surface area is 30.5m
2/ g.
Table 1 adds the size ratio surface-area that different amount an ammonium nitrate have obtained particle surface Zeta potential and product
| Zeta potential (ev) | Product granularity D 50(μm) | Specific surface (m 2/g) | Pattern | |
| Comparative Examples 1 Comparative Examples 2 |
- - -2.4 -8.2 -15.7 | 451097.580.245.5 | 919.54751.870.5 | Irregular spherical Polygons particle is spherical spherical |
| Embodiment 4 | -18.0 | 34.0 | 91.6 | Spherical |
Table 2 ammonium chloride add-on is to the influence of particle surface Zeta potential, product granularity and surface-area
| Zeta potential (ev) | Product granularity D 50(μm) | Specific surface (m 2/g) | | |
| Embodiment | ||||
| 5 embodiment 6 | -23.4 -34.4 | 42.2 30.3 | 20.6 33.3 | Spherical |
| Embodiment 7 | -40.0 | 28.5 | 45.6 | Spherical |
Claims (9)
1. the preparation method of a volume particle size, large specific surface spherical yttrium oxide; It is characterized in that, in precipitation process, control raw material ratio, and regulate the size of product granularity and specific surface through the solubility ammonium salt that adds different amounts; The slurries ageing of post precipitation; Filter, calcining obtains volume particle size, large specific surface spherical yttrium oxide, and concrete steps are following:
(1) adopting the inorganic salt solution of yttrium is raw material; Under certain temperature stirs, add ammonium bicarbonate soln and precipitate, the add-on of described bicarbonate of ammonia is the 100%-300% of theoretical consumption; Obtain containing the slurries of yttrium carbonate particle, the precipitation reaction temperature in the step (1) is 15-40 ℃;
(2) behind reinforced the finishing; In slurries, add the solubility ammonium salt, stir, add the granularity that the ammonium salt amount is adjusted yttrium oxide through adjustment; Described solubility ammonium salt is one or more in ammonium chloride, an ammonium nitrate and the ammonium sulfate, and add-on is for greater than 0 and be less than or equal to 3mol/L;
(3) stop to stir, slurries are ageing at a certain temperature, keeps in the ageing process leaving standstill, and temperature was 15-40 ℃ when slurries were still aging;
(4) slurries after the ageing are through filtering, wash, calcining, and the yttrium oxide the finished product particle that obtains is spherical in shape, and granularity and specific surface area are respectively at D
50=20-100 μ m and 10-100m
2In/g the scope.
2. preparation method according to claim 1 is characterized in that, the inorganic salt solution of yttrium is one or both mixing in Yttrium trinitrate, the Yttrium trichloride in the step (1), and concentration is 0.5-2.0mol/L.
3. preparation method according to claim 1 and 2 is characterized in that, the concentration 0.5-2.0mol/L of ammonium bicarbonate soln in the step (1).
4. preparation method according to claim 1 and 2 is characterized in that, the add-on of described bicarbonate of ammonia is the 105%-120% of theoretical consumption.
5. preparation method according to claim 1 is characterized in that, described precipitation reaction temperature is 20-30 ℃.
6. preparation method according to claim 1 is characterized in that, temperature was 25-30 ℃ when described slurries were still aging.
7. preparation method according to claim 1 is characterized in that, step (3) the still aging time of described slurries is 6-60 hour.
8. preparation method according to claim 7 is characterized in that, step (3) the still aging time of described slurries is 12-48 hour.
9. preparation method according to claim 1 is characterized in that, the described calcining temperature of step (4) is 600 ℃-1100 ℃.
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| CN103449816B (en) * | 2013-08-06 | 2015-02-11 | 施丽萍 | Plasma-etching-resistant granulated yttrium oxide for hot spraying and preparation method thereof |
| CN103936051A (en) * | 2014-05-05 | 2014-07-23 | 包头稀土研究院 | Method for preparing large-grained yttria by virtue of adding NH4Cl into material liquid |
| CN104445350A (en) * | 2014-12-12 | 2015-03-25 | 广西科技大学 | Superfine Y2O3 powder prepared by adopting ultrasonically-assisted precipitation method |
| CN105645455B (en) * | 2016-01-04 | 2017-11-17 | 东北大学 | A kind of method that superfine nano powder is prepared using pulse current |
| CN106082296A (en) * | 2016-06-08 | 2016-11-09 | 广西科技大学 | A kind of spherical yttrium oxide raw powder's production technology |
| CN109616308B (en) * | 2018-11-07 | 2020-09-04 | 湖北第二师范学院 | Magnetic powder extracted from spherical nanometer iridium oxide DNA and production method thereof |
| CN109366039B (en) * | 2018-11-27 | 2020-08-04 | 浙江大学 | Preparation method of yttrium oxide microspheres for titanium alloy vacuum brazing flow inhibitor |
| CN113173593A (en) * | 2021-05-17 | 2021-07-27 | 西南石油大学 | Preparation method of stable nano yttrium oxide powder |
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| CN1061402A (en) * | 1990-11-13 | 1992-05-27 | 罗纳·布朗克化学公司 | The production method of double oxalate of rare earth ammonium and be used for producing rare earth oxide |
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