CN1433968A - Process for preparing nano barium carbonate powder material - Google Patents
Process for preparing nano barium carbonate powder material Download PDFInfo
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- CN1433968A CN1433968A CN 02109077 CN02109077A CN1433968A CN 1433968 A CN1433968 A CN 1433968A CN 02109077 CN02109077 CN 02109077 CN 02109077 A CN02109077 A CN 02109077A CN 1433968 A CN1433968 A CN 1433968A
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- barium
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- carbonate powder
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Abstract
The present invention uses BaCl2 and H2TiO2 as main raw material, and adopts the following steps: utilizing strong oxidant to make catalysis, adding ammonia water to regulate pH value to about 12, filtering to obtain BaTiO3 solution, placing said solution into a high-temp. and high pressure reactor still to make treatment, its treatment temp. is at 300 deg.C-400 deg.C and treatment pressure is 15-22 mPa, cooling and vacuum drying so as to obtain the invented nano-grade barium titanate powder material.
Description
Technical field
The present invention relates to nano barium carbonate powder material and preparation method thereof.
Background technology
The nano barium phthalate material is a kind of nano level titanate powder material, grain-size is between 20～60nm, appearance color is a white, it is the important foundation raw material of electrode component, be mainly used in media ceramic, the manufacturing of sensitive ceramic, laminated ceramic capacitor wherein, the PTC themistor part is widely used, the PTC thermistor is at the refrigerator starter, color TV magnet exterminator, program-controlled telephone, electricity-saving lamp, fields such as well heater have a wide range of applications, the MLC multi-layer ceramic capacitance is widely used aspect large-scale integrated circuit, the barium-titanate material particle diameter has remarkable influence for the performance of sintering barium titanate ceramics and barium titanate ceramics itself, as: barium titanate particle diameter when the 20nm, the comparable particle diameter of the sintering temperature of barium titanate ceramics descends when 20um about 100 ℃, and sintered density improves greatly, as seen, nano level metatitanic acid barium material has crucial effects to the character of barium titanate ceramics.At present, the preparation method of powder level barium-titanate material of receiving has four kinds, sol-gel processing, colloidal sol-precipitator method, stearate method, coprecipitation method, the common drawback of these four kinds of methods is material cost height, reaction efficiency is low, production efficiency is low, produce into thing is difficult for separating controlling, impurity is many, and the difficulty of industrialization is strengthened.
Summary of the invention
The purpose of this invention is to provide a kind of with low cost, production efficiency height, final product rate height, the preparation method of the nano barium carbonate powder material that impurity is few.
Technical solution of the present invention is, adopt high-temperature high pressure water thermal synthesis-coprecipitation method in autoclave, to produce, earlier in solubility barium ion salts solution, add metatitanic acid, add strong oxidizer again, evenly stir simultaneously, stir after 20 minutes, add ammonia soln the pH value is adjusted to 11～13, throw out is carried out vacuum filtration, obtains the barium titanate throw out, then with deionized water wash to the pH value 8～10, soak into 2h with tensio-active agent again, barium titanate solution is put into reactor, be heated to 300～400 ℃, be forced into 15～22mP and handle, time 4～5hr, obtain after the cooling with barium titanate nano particle liquid, carry out vacuum-drying, finally obtain nano level barium titanate powder powder material.
Soluble barium salt BaCl in the starting material
2Be 48～52%, metatitanic acid H
2Tio
3Be 52～48%.
Solubility barium ion concentration of salt solution with the deionized water preparation is 0.4M.
Mole such as the amount of metatitanic acid and solubility barium ion salts solution.
Strong oxidizer is H
2O
2
The invention has the beneficial effects as follows, with low cost, the production efficiency height, final product rate height, impurity is few, thereby more adapts to the demand for development of industrialization.
Embodiment
The present invention is further illustrated below in conjunction with embodiment,
Take by weighing the BaCl of 6.38kg, 27mol
2, put into reactor, in container, add deionized water, evenly be mixed with the Ba of 0.27mol with magnetic stirring apparatus
2+Salts solution is standby, adds the H of 2.12kg, 27mol
2Tio
3, slowly add 40% hydrogen peroxide, evenly stir after 20 minutes simultaneously, add 30% ammoniacal liquor and regulate the pH value 12, treat sediment B aTio
3Generate, carry out vacuum filtration, obtain the barium titanate filter cake, then with deionized water wash to pH value to 9, carrying out twice alcohol with Virahol washes, above-mentioned solution is inserted in the high-temperature high-pressure reaction kettle, heat, be forced into 18mPa and react 4hr to 350 ℃, after the cooling, the barium titanate nano particle,colloid that obtains is carried out vacuum-drying, finally obtain nano level barium titanate powder powder material, its particle diameter is below 20nm.
Claims (5)
1. the preparation method of nano barium carbonate powder material, it is characterized in that, earlier in solubility barium ion salts solution, add metatitanic acid, add strong oxidizer again, evenly stir simultaneously, stir after 20 minutes, add ammonia soln the pH value is adjusted to 11～13, throw out is carried out vacuum filtration, obtains the barium titanate throw out, then with deionized water wash to the pH value 8～10, soak into 2h with tensio-active agent again, barium titanate solution is put into reactor, be heated to 300～400 ℃, be forced into 15～22mP and handle, time 4～5hr, obtain barium titanate nano particle liquid after the cooling, carry out vacuum-drying, finally obtain nano level barium titanate powder powder material.
2. the preparation method of nano barium carbonate powder material according to claim 1 is characterized in that, soluble barium salt BaCl in the starting material
2Be 48～52%, metatitanic acid H
2Tio
3Be 52～48%.
3. the preparation method of nano barium carbonate powder material according to claim 1 is characterized in that, the solubility barium ion concentration of salt solution of preparing with deionized water is 0.4M.
4. the preparation method of nano barium carbonate powder material according to claim 1 is characterized in that, mole such as the amount of metatitanic acid and solubility barium ion salts solution.
5. the preparation method of nano barium carbonate powder material according to claim 1 is characterized in that, strong oxidizer is H
2O
2
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02109077 CN1240618C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano barium carbonate powder material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02109077 CN1240618C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano barium carbonate powder material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1433968A true CN1433968A (en) | 2003-08-06 |
| CN1240618C CN1240618C (en) | 2006-02-08 |
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ID=27628052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02109077 Expired - Fee Related CN1240618C (en) | 2002-01-22 | 2002-01-22 | Process for preparing nano barium carbonate powder material |
Country Status (1)
| Country | Link |
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| CN (1) | CN1240618C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734125A (en) * | 2018-12-28 | 2019-05-10 | 南通奥新电子科技有限公司 | A method of preparing nanostructure metatitanic acid barium |
-
2002
- 2002-01-22 CN CN 02109077 patent/CN1240618C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734125A (en) * | 2018-12-28 | 2019-05-10 | 南通奥新电子科技有限公司 | A method of preparing nanostructure metatitanic acid barium |
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| Publication number | Publication date |
|---|---|
| CN1240618C (en) | 2006-02-08 |
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