CN111017980A - Preparation method of high-purity nano lanthanum oxide material - Google Patents
Preparation method of high-purity nano lanthanum oxide material Download PDFInfo
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- CN111017980A CN111017980A CN201911360954.2A CN201911360954A CN111017980A CN 111017980 A CN111017980 A CN 111017980A CN 201911360954 A CN201911360954 A CN 201911360954A CN 111017980 A CN111017980 A CN 111017980A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a preparation method of a high-purity nano lanthanum oxide material, which comprises the steps of mixing lanthanum chloride and deionized water according to a ratio to prepare a precursor material liquid, adding an active dispersing agent into the precursor material liquid in a reaction kettle, heating, keeping the temperature, reacting, filtering to prepare a high-purity wet nano lanthanum oxide material, and finally carrying out cyclone flash evaporation drying on the high-purity wet nano lanthanum oxide material to obtain the high-purity dry nano lanthanum oxide powder. The purity of the nano lanthanum oxide dry powder prepared by the preparation method can reach 99.99 percent, and the particle size of the powder is more uniform.
Description
Technical Field
The invention relates to a preparation method of a high-purity nano lanthanum oxide material, belonging to the field of fine chemical engineering.
Background
The nanometer lanthanum oxide is white solid powder, has molecular weight of 325.8091, melting point of 2315 ℃ and boiling point of 4200 ℃, is mainly used for manufacturing precision optical glass and optical fiber, is also used as ceramic capacitor in electronic industry, is used as piezoelectric ceramic doping agent, and is also used as raw material for preparing lanthanum boride, petroleum separation and refining catalyst, etc. The existing preparation process for preparing nano lanthanum oxide has low purity of nano lanthanum oxide, so a method for preparing high-purity nano lanthanum oxide is needed to improve the purity of the nano lanthanum oxide.
Disclosure of Invention
In order to realize the technical purpose, the invention provides a preparation method of a high-purity nano lanthanum oxide material, which adopts the technical scheme that:
a preparation method of a high-purity nano lanthanum oxide material comprises the following steps:
(1) preparing precursor liquid: lanthanum chloride and deionized water are mixed according to a certain proportion to prepare a lanthanum chloride solution, and precursor feed liquid is obtained.
(2) Preparing a high-purity nano lanthanum oxide wet material: adding the precursor liquid into a reaction kettle, adding an active dispersant, stirring uniformly, slowly adding liquid ammonia, adjusting the pH to 8-11, heating to 60-250 ℃, reacting for 50-90 h while keeping the temperature, cooling to room temperature, and filtering to obtain the high-purity wet nano lanthanum oxide material.
(3) Preparing high-purity nano lanthanum oxide dry powder: carrying out cyclone flash drying on the high-purity nano lanthanum oxide wet material, and introducing high-purity N into a cyclone flash drying device2And heating the gas to 650-1000 ℃, preserving the heat for 1-3.5 h, and cooling to obtain the high-purity nano lanthanum oxide dry powder.
Preferably, in the step (1), the mass ratio of the lanthanum chloride to the deionized water is 1: 1.5-5.5.
Preferably, the active dispersant added in step (2) includes polyethylene glycol active dispersants, alcohol active dispersants and alcohol ether active dispersants.
Preferably, in the step (2), the adding speed of the liquid ammonia is 1-20 kg/min.
Preferably, in the step (2), the heating rate of the reaction kettle is 2-6 ℃/min.
Preferably, in the step (3), the heating rate is 3.5-8.5 ℃/min.
The invention has the beneficial effects that: the purity of the nano lanthanum oxide dry powder prepared by the preparation method is high and can reach 99.99%, and the particle size of the prepared nano lanthanum oxide powder is more uniform.
Detailed Description
The preparation process of the present invention will be further described with reference to examples.
Example (b):
a preparation method of a high-purity nano lanthanum oxide material comprises the following steps:
(1) preparing precursor liquid: lanthanum chloride and deionized water are mixed according to the mass ratio of 1:5 to prepare a lanthanum chloride solution, and precursor feed liquid is obtained.
(2) Preparing a high-purity nano lanthanum oxide wet material: adding the precursor liquid into a reaction kettle, simultaneously adding active dispersing agents polyethylene glycol 400, methyl amyl alcohol and dodecyl alcohol ether, uniformly stirring, adding liquid ammonia at the speed of 1.5kg/min, regulating the pH value to 8.5, heating to 108 ℃ at the speed of 5 ℃/min, carrying out heat preservation reaction for 60h, cooling to room temperature, carrying out first-step coarse filtration by using a filter screen, second-step fine filtration by using a filter, and fine filtration by using a nanofiltration membrane to obtain the high-purity nano lanthanum oxide wet material.
(3) Preparing high-purity nano lanthanum oxide dry powder: and (3) carrying out cyclone flash drying on the high-purity nano lanthanum oxide wet material, introducing high-purity N2 gas into cyclone flash drying equipment, heating to 820 ℃ at the speed of 7 ℃/min, preserving heat for 1.5h, and cooling to obtain the high-purity nano lanthanum oxide dry powder.
Tests prove that the purity of the nano lanthanum oxide dry powder prepared by the embodiment can reach 99.99 percent, and the particle size of the powder is more uniform.
Claims (6)
1. A preparation method of a high-purity nano lanthanum oxide material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing precursor liquid: mixing lanthanum chloride and deionized water according to a certain proportion to prepare a lanthanum chloride solution, namely a precursor feed liquid;
(2) preparing a high-purity nano lanthanum oxide wet material: adding the precursor liquid into a reaction kettle, adding an active dispersant, stirring uniformly, slowly adding liquid ammonia, adjusting the pH to 8-11, heating to 60-250 ℃, reacting for 50-90 h while keeping the temperature, cooling to room temperature, and filtering to obtain a high-purity wet nano lanthanum oxide material;
(3) preparing high-purity nano lanthanum oxide dry powder: carrying out cyclone flash drying on the high-purity nano lanthanum oxide wet material, and introducing high-purity N into a cyclone flash drying device2And heating the gas to 650-1000 ℃, preserving the heat for 1-3.5 h, and cooling to obtain the high-purity nano lanthanum oxide dry powder.
2. The method for preparing the high-purity nano lanthanum oxide material according to claim 1, which is characterized in that: the mass ratio of the lanthanum chloride to the deionized water in the step (1) is 1: 1.5-5.5.
3. The method for preparing the high-purity nano lanthanum oxide material according to claim 1, which is characterized in that: the active dispersing agent added in the step (2) comprises polyethylene glycol active dispersing agent, alcohol active dispersing agent and alcohol ether active dispersing agent.
4. The method for preparing the high-purity nano lanthanum oxide material according to claim 1, which is characterized in that: and (3) adding the liquid ammonia in the step (2) at a speed of 1-20 kg/min.
5. The method for preparing the high-purity nano lanthanum oxide material according to claim 1, which is characterized in that: and (3) the temperature rising rate of the reaction kettle in the step (2) is 2-6 ℃/min.
6. The method for preparing the high-purity nano lanthanum oxide material according to claim 1, which is characterized in that: and (4) in the step (3), the heating rate is 3.5-8.5 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911360954.2A CN111017980A (en) | 2019-12-26 | 2019-12-26 | Preparation method of high-purity nano lanthanum oxide material |
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| CN201911360954.2A CN111017980A (en) | 2019-12-26 | 2019-12-26 | Preparation method of high-purity nano lanthanum oxide material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394810A (en) * | 2002-06-17 | 2003-02-05 | 施越群 | Preparation method of nano lanthanum oxide |
| CN102161498A (en) * | 2011-06-03 | 2011-08-24 | 北京化工大学 | Preparation method of uniformly dispersed nano lanthanum oxide |
| CN102249283A (en) * | 2011-06-03 | 2011-11-23 | 北京化工大学 | Method for preparing highly-dispersed nano-sized lanthanum oxide by carbon black system |
| CN105948098A (en) * | 2016-04-22 | 2016-09-21 | 广州市威格林环保科技有限公司 | Spherical lanthanum oxide |
| CA3024282A1 (en) * | 2016-05-18 | 2017-11-23 | Rhodia Operations | Cerium oxide particles and method for production thereof |
| CN108557863A (en) * | 2018-05-29 | 2018-09-21 | 淮北师范大学 | A kind of preparation method of lanthana |
-
2019
- 2019-12-26 CN CN201911360954.2A patent/CN111017980A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394810A (en) * | 2002-06-17 | 2003-02-05 | 施越群 | Preparation method of nano lanthanum oxide |
| CN102161498A (en) * | 2011-06-03 | 2011-08-24 | 北京化工大学 | Preparation method of uniformly dispersed nano lanthanum oxide |
| CN102249283A (en) * | 2011-06-03 | 2011-11-23 | 北京化工大学 | Method for preparing highly-dispersed nano-sized lanthanum oxide by carbon black system |
| CN105948098A (en) * | 2016-04-22 | 2016-09-21 | 广州市威格林环保科技有限公司 | Spherical lanthanum oxide |
| CA3024282A1 (en) * | 2016-05-18 | 2017-11-23 | Rhodia Operations | Cerium oxide particles and method for production thereof |
| CN108557863A (en) * | 2018-05-29 | 2018-09-21 | 淮北师范大学 | A kind of preparation method of lanthana |
Non-Patent Citations (1)
| Title |
|---|
| GOHARSHADI ET AL.: ""Influence of preparation methods of microwave, sol–gel, and hydrothermal on structural and optical properties of lanthania nanoparticles"", 《JOURNAL OF THE IRANIAN CHEMICAL SOCIETY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
| CN115231605B (en) * | 2022-07-26 | 2024-02-06 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
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