CN108557864A - A kind of D50:The preparation method and application of the samarium oxide of 7-10um - Google Patents
A kind of D50:The preparation method and application of the samarium oxide of 7-10um Download PDFInfo
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- CN108557864A CN108557864A CN201810569298.6A CN201810569298A CN108557864A CN 108557864 A CN108557864 A CN 108557864A CN 201810569298 A CN201810569298 A CN 201810569298A CN 108557864 A CN108557864 A CN 108557864A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention belongs to Nano Rare-earth Materials preparation fields, are related to a kind of D50:The preparation method and application of the samarium oxide of 7 10um.The samarium trichloride solution of compounding high concentration first in retort, and be stirred；Then the oxalic acid solution of high concentration is added dropwise, it is static after stirring 15min after completion of dropwise addition；60 70 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot；Material mixture liquid is discharged to and is filtered in bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, is filtered dry after washing, obtains sediment；Sediment progress calcination is finally obtained into samarium oxide, is precipitated using high concentration cold water, in conjunction with warm water water-bath, hot water washing, D50 has been made in synergistic effect:The samarium oxide particle of 7 10um.
Description
Technical field
The invention belongs to Nano Rare-earth Materials preparation field, more particularly to a kind of D50:The preparation side of the samarium oxide of 7-10um
Method and application.
Background technology
Rare earth element has unique electron configuration, and the ultrafine powder material of rare earth compound or rare earth oxide is made to have
Many special properties and application.The ultrafine powder material of rare earth oxide is because of its small-size effect, skin effect, quantum size
Effect and macro quanta tunnel effect make ultrafine powder material occur the characteristic that conventional material does not have in terms of light, electricity, magnetic,
Thus by social greatly concern.Samarium oxide ultrafine powder since its huge specific surface area makes it have high catalytic activity,
It can improve the catalytic performance of noble metal catalyst in auto-exhaust catalyst, reduce the dosage of noble metal and reduce cost.
In terms of magnetic material, samarium oxide is mainly for the preparation of rare earth permanent-magnetic material.
The method for preparing samarium oxide has the precipitation method and hydro-thermal method, and hydro-thermal method equipment requirement is higher, and the production time is long, and impurity contains
Amount is high.Common preparation method is the precipitation method, and oxalate precipitation method is the method for inexpensive low impurity and easy expanding production, but general
The samarium oxide particle D50 that makes of oxalate precipitation method do not exceed 3-6um, particle diameter distribution is wider.And usually oxalate precipitation method needs
Ammonium hydroxide is used, but band ammonium ion is unfavorable for environmental protection in ammonium hydroxide.
Invention content
The invention discloses a kind of D50:The preparation method of 7-10um samarium oxides, specific preparation method are：
(1) the samarium trichloride solution that compound concentration is 0.8-1mol/L in retort, wherein retort Ceramics react
Sandwich pot；After stirring 0.5 hour, the oxalic acid solution of a concentration of 0.6-0.8mol/L is added dropwise, it is quiet after stirring 15min after completion of dropwise addition
Set carry out precipitation reaction.
It can make to generate larger samarium oxide particle when reaction using the samarium trichloride solution and oxalic acid solution of high concentration, to
Guarantee can finally reach ideal granularity.
(2) 60-70 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2-3 hours.It is reacted using ceramics
Sandwich pot can preferably control bath temperature, to ensure particle can be made at the uniform velocity to grow into centainly under conditions of warm water water-bath
Particle size range ensures the size distribution of product.
(3) material mixture liquid is discharged to and is filtered in bucket, drain the liquid in material mixture liquid, pure water is added and carries out water
It washes, washing temperature is more than 95 DEG C, and pure water used in water-washing process and the oxide mass ratio being finally prepared are 300:1,
It is filtered dry after washing, obtains sediment.Using the non-rare earth impurity in hot water washing energy preferably cleaning product, it is further ensured that production
The particles size and distribution of product.
(4) sediment is subjected to calcination, the temperature of sediment calcination is 900 DEG C.
D50 produced by the present invention:The samarium oxide of 7-10um is used for MLCC electronic ceramic dielectric materials, this granularity is added
Samarium oxide can be modified MLCC electronic ceramic dielectric materials, the purpose of to realize thin layer ceramic dielectric, large capacity.
Advantageous effect：
(1) ammonium hydroxide need not be added in the present invention during the reaction, and reaction process does not contain ammonium ion, is good for the environment,
Be conducive to expanding production；
(2) use the samarium trichloride solution of high concentration and oxalic acid solution that can make to generate larger samarium oxide particle when reaction,
To ensure that final products can reach desired particle size；
(2) hydro-thermal circulation is carried out after precipitating again, and anti-as reactor progress water-bath using ceramics reaction Sandwich pot
It answers, ensures water-bath in the hydro-thermal circulation temperature range of the present invention, to obtain D50:The samarium oxide particle of 7-10um；
(3) present invention can be mass-produced, and the product of this specified particle size range obtained is situated between for MLCC electronic ceramics
Material has better comprehensive performance.
(4) present invention is precipitated using high concentration cold water, and in conjunction with warm water water-bath, hot water washing, D50 has been made in synergistic effect:
The samarium oxide particle of 7-10um.
Specific implementation mode
Embodiment 1
Present embodiment prepares 4KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.8mol/L samarium trichlorides solution to 28.67L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 105L of 0.6mol/L, rate of addition 5L/min, time for adding 21min are quiet after stirring 15min after completion of dropwise addition
It sets, 70 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2 hours.Material mixture liquid is discharged to suction filtration bucket
It is interior, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 1200L.Washing temperature is more than 95
DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment, it will
Sediment carries out calcination, and the temperature of sediment calcination is 900 DEG C.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
7.969um。
Embodiment 2
Present embodiment prepares 10KG samarium oxide powders using following technical scheme：Compound concentration is in retort
1mol/L samarium trichlorides solution to 57.36L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 198.41L of 0.8mol/L, rate of addition 5L/min, time for adding 40min stir 15min after completion of dropwise addition
After stand, 65 DEG C of hot water circuit 2 hours is added in the interlayer of ceramics reaction Sandwich pot.Material mixture liquid is discharged to suction filtration
In bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 3000L.Washing temperature is more than 95
DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment, it will
Sediment carries out calcination, and the temperature of sediment calcination is 900 DEG C.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
8.582um。
Embodiment 3
Present embodiment prepares 25KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.9mol/L samarium trichlorides solution to 159.32L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, concentration is added dropwise
It is stirred after completion of dropwise addition for the oxalic acid solution 566.89L of 0.7mol/L, rate of addition 5L/min, time for adding 114min
It is stood after 15min, 65 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2 hours.By material mixture liquid blowing
To filtering in bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 7500L.Washing temperature
More than 95 DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry, is sunk after washing
Sediment is carried out calcination by starch, and the temperature of sediment calcination is 900 DEG C.It is through 2000 particle size analyzer of Malvern detection granularity
D50：7.079um.
Comparative example 1
Present embodiment prepares 10KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.3mol/L samarium trichlorides solution to 191.19L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, concentration is added dropwise
It is stirred after completion of dropwise addition for the oxalic acid solution 529.1L of 0.3mol/L, rate of addition 5L/min, time for adding 106min
It is stood after 15min, 65 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2 hours.By material mixture liquid blowing
To filtering in bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 3000L.Washing temperature
More than 95 DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry, is sunk after washing
Sediment is carried out calcination by starch, and the temperature of sediment calcination is 900 DEG C.It is through 2000 particle size analyzer of Malvern detection granularity
D50：3.408um.
Comparative example 2
Present embodiment prepares 10KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.6mol/L samarium trichlorides solution to 95.6L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 264.55L of 0.6mol/L, rate of addition 5L/min, time for adding 52.91min are stirred after completion of dropwise addition
It is stood after 15min, 65 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2 hours.By material mixture liquid blowing
To filtering in bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 3000L.Washing temperature
More than 95 DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry, is sunk after washing
Sediment is carried out calcination by starch, and the temperature of sediment calcination is 900 DEG C.It is through 2000 particle size analyzer of Malvern detection granularity
D50：5.317um.
Comparative example 3
Present embodiment prepares 10KG samarium oxide powders using following technical scheme：Compound concentration is in retort
1.1mol/L samarium trichlorides solution to 52.15L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 144.3L of 1.1mol/L, rate of addition 5L/min, time for adding 29min, after stirring 15min after completion of dropwise addition
It stands, 65 DEG C of hot water circuit is added in the interlayer of ceramics reaction Sandwich pot 2 hours.Material mixture liquid is discharged to suction filtration
In bucket, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 3000L.Washing temperature is more than 95
DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment, it will
Sediment carries out calcination, and the temperature of sediment calcination is 900 DEG C.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
5.878um。
Comparative example 4
Present embodiment prepares 10KG samarium oxide powders using following technical scheme：Compound concentration is in retort
1.5mol/L samarium trichlorides solution to 38.24L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 105.82L of 1.5mol/L, rate of addition 5L/min, time for adding 21min stir 15min after completion of dropwise addition
After stand, 65 DEG C of hot water circuit 2 hours is added in the interlayer of ceramics reaction Sandwich pot.Material mixture liquid is discharged to pumping
In lauter tub, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 3000L.Washing temperature is more than
95 DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment,
Sediment is subjected to calcination, the temperature of sediment calcination is 900 DEG C.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
6.034um。
Comparative example 5
Present embodiment prepares 8KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.8mol/L samarium trichlorides solution is to 57.36L, and with 80 DEG C of hot pure water raw material liquid, retort Ceramics react Sandwich pot；It stirs
After mixing 0.5 hour, the oxalic acid solution 158.73L of a concentration of 0.8mol/L, rate of addition 5L/min is added dropwise, time for adding is
It is stood after stirring 15min after 31.75,65 DEG C of the addition hot water circuit 2 hours in the interlayer of ceramics reaction Sandwich pot.By object
Material mixed liquor, which is discharged to, to be filtered in bucket, and the liquid in material mixture liquid is drained, and pure water is added and is washed, and washing pure water amount is
2400L.Washing temperature is more than 95 DEG C, and it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, water
It is filtered dry after washing, obtains sediment, sediment is subjected to calcination, the temperature of sediment calcination is 900 DEG C.Through Malvern 2000
It is D50 to spend instrument detection granularity：13.670um
Comparative example 6
Present embodiment prepares 8KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.8mol/L samarium trichlorides solution is to 57.36L, and with 60 DEG C of hot pure water raw material liquid, retort Ceramics react Sandwich pot；It stirs
After mixing 0.5 hour, the oxalic acid solution 158.73L of a concentration of 0.8mol/L, rate of addition 5L/min is added dropwise, time for adding is
It is stood after stirring 15min after 31.75,65 DEG C of the addition hot water circuit 2 hours in the interlayer of ceramics reaction Sandwich pot.By object
Material mixed liquor, which is discharged to, to be filtered in bucket, and the liquid in material mixture liquid is drained, and pure water is added and is washed, and washing pure water amount is
2400L.Washing temperature is more than 95 DEG C, and it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, water
It is filtered dry after washing, obtains sediment, sediment is subjected to calcination, the temperature of sediment calcination is 900 DEG C.Through Malvern 2000
It is D50 to spend instrument detection granularity：12.953um
Comparative example 7
Present embodiment prepares 8KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.8mol/L samarium trichlorides solution to 57.36L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 158.73L of 0.8mol/L, rate of addition 5L/min, time for adding 31.75min, after stir 15min after
It stands, 80 DEG C of the addition hot water circuit 2 hours in the interlayer of ceramics reaction Sandwich pot.Material mixture liquid is discharged to suction filtration bucket
It is interior, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 2400L.Washing temperature is more than 95
DEG C, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment, it will
Sediment carries out calcination, and the temperature of sediment calcination is 900 DEG C.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
11.985um
Comparative example 8
Present embodiment prepares 8KG samarium oxide powders using following technical scheme：Compound concentration is in retort
0.8mol/L samarium trichlorides solution to 57.36L, retort Ceramics react Sandwich pot；After stirring 0.5 hour, it is added dropwise a concentration of
The oxalic acid solution 158.73L of 0.8mol/L, rate of addition 5L/min, time for adding 31.75min, after stir 15min after
It stands, 60 DEG C of the addition hot water circuit 2 hours in the interlayer of ceramics reaction Sandwich pot.Material mixture liquid is discharged to suction filtration bucket
It is interior, the liquid in material mixture liquid is drained, pure water is added and is washed, washing pure water amount is 2400L.Washing temperature is that room temperature is pure
Water, it is 300 to wash pure water used and the oxide mass ratio being finally prepared:1, it is filtered dry after washing, obtains sediment, it will
Sediment carries out calcination, and the temperature of sediment calcination is 900 degree.It is D50 through 2000 particle size analyzer of Malvern detection granularity：
6.716um。
Claims (7)
1. a kind of D50:The preparation method of 7-10um samarium oxides, it is characterised in that：The preparation method is that：
(1) samarium trichloride solution is prepared in ceramics react Sandwich pot, and be stirred；
(2) oxalic acid solution is added dropwise into the samarium trichloride solution of step (1), is stood after stirring 15min after completion of dropwise addition；
(3) circulating hot water is added in the interlayer of ceramics reaction Sandwich pot and carries out water-bath, obtain mixed liquor；
(4) mixed liquor of step (3) is discharged to and is filtered in bucket, drain the liquid in mixed liquor, pure water is added and is washed, water
It is filtered dry after washing, obtains sediment；
(5) sediment is subjected to calcination.
2. D50 as described in claim 1:The preparation method of 7-10um samarium oxides, it is characterised in that：Step (1) described chlorination
Samarium solution it is a concentration of：0.8-1mol/L；Mixing time is 0.5 hour.
3. D50 as described in claim 1:The preparation method of 7-10um samarium oxides, it is characterised in that：Step (2) described dropwise addition
Oxalic acid solution it is a concentration of：0.6-0.8mol/L.
4. D50 as described in claim 1:The preparation method of 7-10um samarium oxides, it is characterised in that：Step (3) described addition
Circulating hot water be 60-70 DEG C, water bath time is：2-3h.
5. D50 as described in claim 1:The preparation method of 7-10um samarium oxides, it is characterised in that：Step (4) described washing
More than 95 DEG C, the mass ratio of pure water used in water-washing process and the samarium oxide being finally prepared is temperature：300:1.
6. D50 as described in claim 1:The preparation method of 7-10um samarium oxides, it is characterised in that：Step (5) described precipitation
The temperature of object calcination is：900℃.
7. a kind of application of the samarium oxide prepared such as any one of claim 1-6 the methods, it is characterised in that：The samarium oxide
For MLCC electronic ceramic dielectric materials.
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Citations (7)
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| CN101186327A (en) * | 2006-11-16 | 2008-05-28 | 北京方正稀土科技研究所有限公司 | Large granularity high apparent density rare earth oxide and preparation method thereof |
| CN101306828A (en) * | 2007-05-17 | 2008-11-19 | 北京有色金属研究总院 | Device and process for preparing rare-earth compound uniform micro powder |
| CN104419839A (en) * | 2013-08-19 | 2015-03-18 | 中铝稀土（常州）有限公司 | Method for preparing rare earth oxalate precipitation |
| CN104446468A (en) * | 2014-11-30 | 2015-03-25 | 桂林理工大学 | X9R ceramic capacitor dielectric material and preparation method thereof |
| CN106006701A (en) * | 2016-05-19 | 2016-10-12 | 福建省长汀金龙稀土有限公司 | Preparation method of micron-submicron-scale rare earth oxide powder |
| CN106044834A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of 1-2-micron samarium oxide |
-
2018
- 2018-06-05 CN CN201810569298.6A patent/CN108557864A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63182216A (en) * | 1987-01-20 | 1988-07-27 | Daido Steel Co Ltd | Method for separation and recovery of rare earth element |
| CN101186327A (en) * | 2006-11-16 | 2008-05-28 | 北京方正稀土科技研究所有限公司 | Large granularity high apparent density rare earth oxide and preparation method thereof |
| CN101306828A (en) * | 2007-05-17 | 2008-11-19 | 北京有色金属研究总院 | Device and process for preparing rare-earth compound uniform micro powder |
| CN104419839A (en) * | 2013-08-19 | 2015-03-18 | 中铝稀土（常州）有限公司 | Method for preparing rare earth oxalate precipitation |
| CN104446468A (en) * | 2014-11-30 | 2015-03-25 | 桂林理工大学 | X9R ceramic capacitor dielectric material and preparation method thereof |
| CN106006701A (en) * | 2016-05-19 | 2016-10-12 | 福建省长汀金龙稀土有限公司 | Preparation method of micron-submicron-scale rare earth oxide powder |
| CN106044834A (en) * | 2016-06-07 | 2016-10-26 | 福建省长汀金龙稀土有限公司 | Preparation method of 1-2-micron samarium oxide |
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