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Method for preparing platy lanthanum hydroxide nanocrystalline through microwave-ultrasonic method

A technology of lanthanum hydroxide and ultrasonic method, applied in chemical instruments and methods, nanotechnology, inorganic chemistry, etc., can solve the problems of long reaction time under experimental conditions, poor product dispersibility, small specific surface area of ​​samples, etc., and achieve dispersibility Good, short reaction time cycle, excellent performance effect

Inactive Publication Date: 2013-02-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for preparing lanthanum hydroxide mainly include solvothermal method [Hou B, Xu Y, Wu D, et al.Synthesis and characterization of ultralong lanthanum hydroxide[J].J Mater Sci, 2007(42):1397-1400.], It is easy to obtain pure phase nanomaterials, but the dispersion of the product is not good; the traditional hydrothermal method [Ma X, Zhang H, Ji Y, et al.Synthesis of ultrafine lanthanum hydroxide nanorods by a simple hydrothermal process[J].MaterLett , 2004(58):1180-1182.] needs to be carried out in the reactor at high temperature and high pressure, requiring strict experimental conditions and relatively long reaction time; precipitation method [Zhou Yang, Chen Shuguang, etc. Simple precipitation method to prepare lanthanum hydroxide nanorods and its structural characterization[J].Journal of Changsha University of Science and Technology.2009.6(4):8589]The specific surface area of ​​the prepared sample is small, and the product uniformity is not good

Method used

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  • Method for preparing platy lanthanum hydroxide nanocrystalline through microwave-ultrasonic method
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Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1) Analytical pure lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.05mol / L;

[0021] 2) Add analytically pure polyethylene glycol (PEG) to solution A so that the concentration of PEG in the solution is 0.005mol / L to obtain solution B;

[0022] 3) Add potassium hydroxide or sodium hydroxide solution to solution B to make La 3+ / OH - The molar ratio of is 1:10, magnetic stirring forms precursor solution C;

[0023] 4) Pour the precursor solution C into a four-neck round bottom flask, put it into the UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis reaction instrument, select the combination of microwave heating and ultrasonic wave in the temperature-time mode, the temperature -The temperature of the time mode is controlled at 160°C, the reaction time is controlled at 120min, and naturally cooled to room temperature after the reaction;

[0024] 5) The product was coll...

Embodiment 2

[0026] 1) Analytical pure lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.1mol / L;

[0027] 2) Add analytically pure polyethylene glycol (PEG) to solution A so that the concentration of PEG in the solution is 0.007mol / L to obtain solution B;

[0028] 3) Add potassium hydroxide or sodium hydroxide solution to solution B to make La 3+ / OH - The molar ratio of is 1:15, magnetic stirring forms precursor solution C;

[0029] 4) Pour the precursor solution C into a four-neck round bottom flask, put it into the UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis reaction instrument, select the combination of microwave heating and ultrasonic wave in the temperature-time mode, the temperature -The temperature in the time mode is controlled at 180°C, the reaction time is controlled at 100min, and naturally cooled to room temperature after the reaction;

[0030] 5) The product was colle...

Embodiment 3

[0032] 1) Analytical pure lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.5mol / L;

[0033] 2) Add analytically pure polyethylene glycol (PEG) to solution A so that the concentration of PEG in the solution is 0.008mol / L to obtain solution B;

[0034] 3) Add potassium hydroxide or sodium hydroxide solution to solution B to make La 3+ / OH - The molar ratio of is 1:20, magnetic stirring forms precursor solution C;

[0035] 4) Pour the precursor solution C into a four-neck round bottom flask, put it into the UWave-1000 microwave-ultraviolet-ultrasonic trinity synthesis reaction instrument, select the combination of microwave heating and ultrasonic wave in the temperature-time mode, the temperature -The temperature of the time mode is controlled at 200°C, the reaction time is controlled at 80 minutes, and naturally cooled to room temperature after the reaction;

[0036] 5) The product was c...

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Abstract

The invention provides a method for preparing platy lanthanum hydroxide nanocrystalline through a microwave-ultrasonic method. Analytically pure lanthanum nitrate hexahydrate and polyethylene glycol are added in deionized water to obtain a solution B; a potassium hydroxide or sodium hydroxide solution is added in the solution B to form a precursor solution C; the precursor solution C is poured into a four-neck round-bottom flask, the flask is put in a microwave-ultraviolet-ultrasonic trinity synthesis reaction apparatus, microwave heating and ultrasonic combination under a temperature-time mode is selected, the precursor solution C is cooled to the room temperature naturally after reaction is finished, a product is collected through centrifugation and then washed several times by deionized water and absolute ethyl alcohol, and the product is dried to obtain the final product platy lanthanum hydroxide nanocrystalline. The method adopts a simple microwave-ultrasonic preparation process, is short in reaction time period and low in energy consumption, reaction can be finished in liquid phase in one time, and no after-treatment is needed. La(OH)3 particles made by the method are of platy structures and are large in specific surface area, good in dispersibility and excellent in performance.

Description

technical field [0001] The invention relates to a preparation method of lanthanum hydroxide, in particular to a method for preparing sheet-shaped lanthanum hydroxide nanocrystals by a microwave-ultrasonic method. technical background [0002] As an important strategic resource, rare earth is widely used in various fields of the national economy. It significantly improves the benefits of industries such as metallurgy, petrochemical, machinery, agriculture, forestry, animal husbandry and fishery, and creates dozens or hundreds of times the value of rare earth itself. Scientists call it a "treasure trove of new materials." Lanthanum Hydroxide La(OH) 3 With excellent optical, electrical, and magnetic properties, it has been widely used as a catalyst, adsorbent, fluorescent agent, time-resolved fluorescence (TRF) biolabel, and the above-mentioned conversion materials. Nanostructured materials exhibit many properties superior to their bulk counterparts due to quantum size effect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00B82Y40/00
Inventor 黄剑锋符馨元曹丽云吴建鹏李翠艳卢静
Owner SHAANXI UNIV OF SCI & TECH
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