CN106745206A - The method of solvent hot preparation nano barium carbonate powder - Google Patents
The method of solvent hot preparation nano barium carbonate powder Download PDFInfo
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- CN106745206A CN106745206A CN201611068059.XA CN201611068059A CN106745206A CN 106745206 A CN106745206 A CN 106745206A CN 201611068059 A CN201611068059 A CN 201611068059A CN 106745206 A CN106745206 A CN 106745206A
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- carbonate powder
- barium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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Abstract
The present invention relates to technical field of function materials, and in particular to a kind of method of solvent hot preparation nano barium carbonate powder.The method of solvent hot preparation nano barium carbonate powder, comprises the following steps：Prepare Ba (OH)2Solution；Prepare white Ti (OH)4 Colloidal sol；By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, and mixing speed is 1200r/min, while being passed through N2Protection 30min, with the air in replacement reaction kettle；200 DEG C are warming up to the speed of 2 DEG C/min after stirring, 0.5 ~ 2h is incubated, using the barium titanate slurry that generation is taken out after cooling water quick cooling；Barium titanate slurry is inserted in special beaker, Ceramic excessive filtration film device is pumped into after dilution, concentrated after circulation washing to filtrate pH value=7 ~ 8, centrifugal spray drying is made nano barium carbonate powder.Technical solution of the present invention is simple, and the nano barium carbonate powder particle diameter being made is small, narrower particle size distribution and with Tetragonal crystallinity higher.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of side of solvent hot preparation nano barium carbonate powder
Method.
Background technology
Barium titanate, especially tetragonal-phase barium titanate are normal with dielectric high as a kind of electron ceramic material of function admirable
The features such as number, low-dielectric loss, there are excellent ferroelectricity, piezoelectricity, pressure-resistant and insulating properties, be widely used in positive temperature coefficient heat
Quick resistance (PTC), thermoelectric element, piezoelectric ceramics, multilayer ceramic capacitor (MLCC) etc., wherein, BaTiO3In MLCC
It is most widely used.Lighting, multifunction with electronic product, MLCC is also towards miniaturization, the direction hair of high capacity
Exhibition, this MLCC for allowing for preparing more film dielectric layer turns into key point.
The ceramic medium material for preparing MLCC uses is different according to the thickness of casting medium, in order to ensure to make electric capacity
The reliability of device, 5 ~ 10 crystal grain are at least piled up in dielectric thickness direction, and current 2 microns of porcelain films curtain coating has turned into main flow, Shao Shuo
This manufacturer has developed 0.5 microns of casting technologies, this is accomplished by selecting the BaTiO of below particle diameter 100nm3It is prepared by powder
MLCC.However, working as BaTiO3When diameter of particle is less than 100 nanometers, due to the presence of " dimensional effect ".BaTiO3The four of powder
Square rate can be reduced with the reduction of particle diameter, until critical dimension is changed into metastable Emission in Cubic；Lacking in barium carbonate powder
Sunken such as hydroxyl, Ba rooms can also suppress barium carbonate powder to be existed in the form of Tetragonal；And prepare less than 2 microns of porcelain films
, it is necessary to barium carbonate powder has extremely narrow size distribution, uneven particle size can cause to go out in barium titanate dielectric layer MLCC
The abnormal growth of existing hole and crystal grain, influences the electric property of MLCC.
In order to meet the rigors that MLCC is proposed to required barium carbonate powder, increasing researcher's selection colloidal sol-
The synthetic methods such as gel, hydro-thermal, overcritical hydro-thermal, molten-salt growth method, spray pyrolysis, and prepare even-grained nanoscale barium titanate
Powder.But there are problems that both sides is to be solved：One is complicated synthesis technique, with high costs；Two is that the powder for synthesizing is often
Metastable Emission in Cubic is, it is necessary to further treatment could be applied.
The content of the invention
The present invention is directed to propose a kind of method of solvent hot preparation nano barium carbonate powder.
Technical program of the present invention lies in：
The method of solvent hot preparation nano barium carbonate powder, comprises the following steps：
Deionized water is measured, 80 ~ 90 DEG C are preheated to；Weigh Ba (OH)2, in the deionized water being placed in after preheating, magnetic agitation；Treat
Ba(OH)2After solid is completely dissolved, vacuum filtration obtains Ba (OH)2Solution；
Respectively weigh butyl titanate, absolute ethyl alcohol, insert in 1L there-necked flasks, under water bath condition magnetic agitation 30 ~
45min；Ammoniacal liquor is measured to be placed in 200mL constant pressure funnels, by ammoniacal liquor instill butyl titanate alcoholic solution in, magnetic agitation 2 ~
2.5h, forms white Ti (OH)4 Colloidal sol；
By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, while being passed through N2
Protection 30min, with the air in replacement reaction kettle；200 DEG C are at the uniform velocity warming up to after stirring, using taking-up after cooling water quick cooling
The barium titanate slurry of generation；Barium titanate slurry is inserted in beaker, Ceramic excessive filtration film device, circulation washing to filter are pumped into after dilution
Concentrated behind liquid pH value=7 ~ 8, spray drying is made nano barium carbonate powder.
The mass concentration of described ammoniacal liquor is 25%.
Described mixing speed is 1200r/min, and mixing time is 1 ~ 1.5h.
The described speed at the uniform velocity heating up is to be warming up to 200 DEG C with the speed of 2 ~ 5 DEG C/min, is incubated 0.5 ~ 2h.
Described spray drying is centrifugal spray drying.
The technical effects of the invention are that：
Technical solution of the present invention is simple, and the nano barium carbonate powder particle diameter being made is small, narrower particle size distribution and with higher four
Square phase crystallinity.
Specific embodiment
The method of solvent hot preparation nano barium carbonate powder, comprises the following steps：
Embodiment 1
Deionized water is measured, 80 ~ 90 DEG C are preheated to；Weigh Ba (OH)2, in the deionized water being placed in after preheating, magnetic agitation；Treat
Ba(OH)2After solid is completely dissolved, vacuum filtration obtains Ba (OH)2Solution；
Respectively weigh butyl titanate, absolute ethyl alcohol, insert in 1L there-necked flasks, under water bath condition magnetic agitation 30 ~
45min；Ammoniacal liquor is measured to be placed in 200mL constant pressure funnels, by ammoniacal liquor instill butyl titanate alcoholic solution in, magnetic agitation 2 ~
2.5h, forms white Ti (OH)4 Colloidal sol；
By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, while being passed through N2
Protection 30min, with the air in replacement reaction kettle；200 DEG C are at the uniform velocity warming up to after stirring, using taking-up after cooling water quick cooling
The barium titanate slurry of generation；Barium titanate slurry is inserted in beaker, Ceramic excessive filtration film device, circulation washing to filter are pumped into after dilution
Concentrated behind liquid pH value=7 ~ 8, spray drying is made nano barium carbonate powder.
Embodiment 2
Deionized water is measured, 80 ~ 90 DEG C are preheated to；Weigh Ba (OH)2, in the deionized water being placed in after preheating, magnetic agitation；Treat
Ba(OH)2After solid is completely dissolved, vacuum filtration obtains Ba (OH)2Solution；
Respectively weigh butyl titanate, absolute ethyl alcohol, insert in 1L there-necked flasks, under water bath condition magnetic agitation 30 ~
45min；Ammoniacal liquor is measured to be placed in 200mL constant pressure funnels, by ammoniacal liquor instill butyl titanate alcoholic solution in, magnetic agitation 2 ~
2.5h, forms white Ti (OH)4 Colloidal sol；
By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, while being passed through N2
Protection 30min, with the air in replacement reaction kettle；200 DEG C are at the uniform velocity warming up to after stirring, using taking-up after cooling water quick cooling
The barium titanate slurry of generation；Barium titanate slurry is inserted in beaker, Ceramic excessive filtration film device, circulation washing to filter are pumped into after dilution
Concentrated behind liquid pH value=7 ~ 8, spray drying is made nano barium carbonate powder.
Wherein, the mass concentration of described ammoniacal liquor is 25%.Described mixing speed is 1200r/min, and mixing time is 1
~1.5h.The described speed at the uniform velocity heating up is to be warming up to 200 DEG C with the speed of 2 ~ 5 DEG C/min, is incubated 0.5 ~ 2h.Described spray
It is centrifugal spray drying that mist is dried.
Embodiment 3
Deionized water is measured, 80 DEG C are preheated to；Weigh Ba (OH)2, in the deionized water being placed in after preheating, magnetic agitation；Treat Ba
(OH)2After solid is completely dissolved, vacuum filtration obtains Ba (OH)2Solution；
Butyl titanate, absolute ethyl alcohol are weighed respectively, are inserted in 1L there-necked flasks, the magnetic agitation 30min under water bath condition；
Measure ammoniacal liquor to be placed in 200mL constant pressure funnels, by ammoniacal liquor instillation butyl titanate alcoholic solution, magnetic agitation 2h forms white
Ti(OH)4 Colloidal sol；
By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, while being passed through N2
Protection 30min, with the air in replacement reaction kettle；200 DEG C are at the uniform velocity warming up to after stirring, using taking-up after cooling water quick cooling
The barium titanate slurry of generation；Barium titanate slurry is inserted in beaker, Ceramic excessive filtration film device, circulation washing to filter are pumped into after dilution
Concentrated behind liquid pH value=7 ~ 8, spray drying is made nano barium carbonate powder.
Wherein, the mass concentration of described ammoniacal liquor is 25%.Described mixing speed is 1200r/min, and mixing time is
1h.The described speed at the uniform velocity heating up is to be warming up to 200 DEG C with the speed of 2 DEG C/min, is incubated 0.5h.Described spray drying
It is centrifugal spray drying.
Claims (5)
1. the method for solvent hot preparation nano barium carbonate powder, it is characterised in that：Comprise the following steps：
Deionized water is measured, 80 ~ 90 DEG C are preheated to；Weigh Ba (OH)2, in the deionized water being placed in after preheating, magnetic agitation；Treat
Ba(OH)2After solid is completely dissolved, vacuum filtration obtains Ba (OH)2Solution；
Respectively weigh butyl titanate, absolute ethyl alcohol, insert in 1L there-necked flasks, under water bath condition magnetic agitation 30 ~
45min；Ammoniacal liquor is measured to be placed in 200mL constant pressure funnels, by ammoniacal liquor instill butyl titanate alcoholic solution in, magnetic agitation 2 ~
2.5h, forms white Ti (OH)4 Colloidal sol；
By the Ba (OH) of above-mentioned preparation2Solution, Ti (OH)4 Colloidal sol is inserted in 1L autoclaves, action of forced stirring, while being passed through N2
Protection 30min, with the air in replacement reaction kettle；200 DEG C are at the uniform velocity warming up to after stirring, using taking-up after cooling water quick cooling
The barium titanate slurry of generation；Barium titanate slurry is inserted in beaker, Ceramic excessive filtration film device, circulation washing to filter are pumped into after dilution
Concentrated behind liquid pH value=7 ~ 8, spray drying is made nano barium carbonate powder.
2. the method for solvent hot preparation nano barium carbonate powder according to claim 1, it is characterised in that：Described ammoniacal liquor
Mass concentration be 25%.
3. the method for solvent hot preparation nano barium carbonate powder according to claim 1, it is characterised in that：Described stirring
Speed is 1200r/min, and mixing time is 1 ~ 1.5h.
4. the method for solvent hot preparation nano barium carbonate powder according to claim 1, it is characterised in that：It is described at the uniform velocity
The speed of intensification is to be warming up to 200 DEG C with the speed of 2 ~ 5 DEG C/min, is incubated 0.5 ~ 2h.
5. the method for solvent hot preparation nano barium carbonate powder according to claim 1, it is characterised in that：Described spraying
It is centrifugal spray drying to dry.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107954469A (en) * | 2017-12-15 | 2018-04-24 | 河北工业大学 | A kind of method for preparing tetragonal phase nano barium titanate |
| CN108160074A (en) * | 2017-12-25 | 2018-06-15 | 扬州大学 | Carry gold BaTiO3The preparation method of photochemical catalyst |
| CN113893841A (en) * | 2021-09-09 | 2022-01-07 | 同济大学 | Barium titanate nano material for piezoelectric catalytic degradation of trace organic pollutants in water and preparation and application thereof |
-
2016
- 2016-11-29 CN CN201611068059.XA patent/CN106745206A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107954469A (en) * | 2017-12-15 | 2018-04-24 | 河北工业大学 | A kind of method for preparing tetragonal phase nano barium titanate |
| CN108160074A (en) * | 2017-12-25 | 2018-06-15 | 扬州大学 | Carry gold BaTiO3The preparation method of photochemical catalyst |
| CN108160074B (en) * | 2017-12-25 | 2020-12-04 | 扬州大学 | Gold-loaded BaTiO3Method for preparing photocatalyst |
| CN113893841A (en) * | 2021-09-09 | 2022-01-07 | 同济大学 | Barium titanate nano material for piezoelectric catalytic degradation of trace organic pollutants in water and preparation and application thereof |
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