Preparation method of bar-shaped lanthanum hydroxide nanocrystal

A technology of lanthanum hydroxide and nanocrystals, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of long reaction time under experimental conditions, poor product dispersion, small specific surface area of ​​samples, etc., and achieve low cost , small grain size and short reaction time period

Active Publication Date: 2014-04-16
上海球球云环保科技有限公司
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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 hydroxidenanorods by a simple hydrothermal process[J].Mater Lett, 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 nano Rod 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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  • Preparation method of bar-shaped lanthanum hydroxide nanocrystal
  • Preparation method of bar-shaped lanthanum hydroxide nanocrystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) The analytically pure lanthanum sulfate nonahydrate (La 2 (SO 4 ) 3 9H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.05mol / L;

[0022] 2) Add analytically pure ethylenediaminetetraacetic acid (EDTA) to solution A so that the concentration of EDTA in the solution is 0.005mol / L to obtain solution B;

[0023] 3) Add 1 mol / L ammonia solution dropwise to solution B to adjust the pH to 8.0, and magnetically stir to form precursor solution C;

[0024] 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 ultraviolet irradiation in the temperature-time mode, the The temperature of the temperature-time mode is controlled at 100°C, the reaction time is controlled at 10 minutes, and naturally cooled to room temperature after the reaction;

[0025] 5) The product was coll...

Embodiment 2

[0027] 1) The analytically pure lanthanum sulfate nonahydrate (La 2 (SO 4 ) 3 9H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.01mol / L;

[0028] 2) Add analytically pure ethylenediaminetetraacetic acid (EDTA) to solution A so that the concentration of EDTA in the solution is 0.01mol / L to obtain solution B;

[0029] 3) Add 1 mol / L ammonia solution dropwise to solution B to adjust the pH to 9.0, and magnetically stir to form precursor solution C;

[0030] 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 ultraviolet irradiation in the temperature-time mode, the The temperature of the temperature-time mode is controlled at 120°C, the reaction time is controlled at 8 minutes, and the reaction is naturally cooled to room temperature after the end of the reaction;

[0031...

Embodiment 3

[0033] 1) The analytically pure lanthanum sulfate nonahydrate (La 2 (SO 4 ) 3 9H 2 O) added to deionized water to make a transparent solution A with a concentration of 0.3mol / L;

[0034] 2) Add analytically pure ethylenediaminetetraacetic acid (EDTA) to solution A so that the concentration of EDTA in the solution is 0.03mol / L to obtain solution B;

[0035] 3) Add 1 mol / L ammonia solution dropwise to solution B to adjust the pH to 10.0, and magnetically stir to form precursor solution C;

[0036] 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 ultraviolet irradiation in the temperature-time mode, the The temperature of the temperature-time mode is controlled at 140 ° C, the reaction time is controlled at 6 minutes, and naturally cooled to room temperature after the reaction is completed;

[0037] 5) The pro...

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Abstract

The invention provides a preparation method of a bar-shaped lanthanum hydroxide nanocrystal. The method comprises the following steps of: adding nona-lanthanum sulfate and ethylenediamine tetraacetic acid into deionized water respectively to obtain a solution B; adjusting the pH of the solution B to 8.0-12.0 with an ammonia water solution to obtain a precursor solution C; pouring the precursor solution C into a four-neck round-bottom flask, putting the four-neck round-bottom flask into a microwave-ultraviolet ray-ultrasonic wave three-in-one synthesis reaction instrument, selecting a microwave heating-ultraviolet irradiation combined reaction in a temperature-time mode, and naturally cooling to the room temperature after the reaction; and centrifugally collecting a product, washing repeatedly with deionized water and absolute ethyl alcohol respectively, and drying to obtain a final product, i.e., bar-shaped lanthanum hydroxide nanocrystal. A simple microwave-ultraviolet ray synthesis method preparation process is adopted, so that the method has the advantages of short reaction time period, low energy consumption, low cost, convenience in operating, one-time completion of a reaction in a liquid phase, and no need of subsequent treatment. La(OH3) particles prepared with the method have bar-shaped structures, are small in size, have high dispersity, and can be applied in the catalysis field and the optics field.

Description

technical field [0001] The invention relates to a preparation method of lanthanum hydroxide, in particular to a preparation method of rod-shaped lanthanum hydroxide nanocrystals. Background technique [0002] Lanthanum Hydroxide La(OH) 3 With excellent optical, electrical, and magnetic properties, it has been widely used as catalysts, adsorbents, fluorescent agents, time-resolved fluorescence (TRF) biolabels, and up-conversion luminescent materials. Nanostructured materials exhibit many properties superior to their bulk counterparts due to quantum size effects. Nanostructured lanthanum hydroxide has a relatively large specific surface area, which can fully contact with the reaction materials and greatly improve its catalytic activity. [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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y30/00
Inventor 曹丽云符馨元黄剑锋费杰李翠艳卢静吴建鹏
Owner 上海球球云环保科技有限公司
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