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Method for preparing multi-morphology nano zinc oxide by solid-phase method

A nano-zinc oxide, multi-morphology technology, applied in the direction of zinc oxide/zinc hydroxide, nanotechnology, nanotechnology, etc., to achieve the effect of easy experimental process, simple process conditions, green and environmental protection yield

Inactive Publication Date: 2020-09-18
淮南前景新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] There are many patents for the preparation of zinc oxide that have been disclosed at present, including: a preparation process of high-purity nano-zinc oxide (publication number: CN109399693A), a preparation method of self-assembled hexagonal prism zinc oxide (publication number: CN109399692A), a Preparation of zinc oxide and particle size control method (publication number: CN109133149A), a preparation method of nano-zinc oxide (publication number: CN108821328A), a preparation method of active zinc oxide (publication number: CN108455656A), feed-grade active oxidation The preparation method of zinc (publication number: CN108467055A), a polyhedral zinc oxide and its preparation method (publication number: CN108163884A), etc., but use solid phase method, especially manual grinding and use basic zinc carbonate as the precursor to synthesize nano oxide Zinc, but few related literature reports

Method used

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  • Method for preparing multi-morphology nano zinc oxide by solid-phase method
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  • Method for preparing multi-morphology nano zinc oxide by solid-phase method

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Experimental program
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Effect test

Embodiment 1

[0041] 1. Weigh 11.52g of zinc sulfate heptahydrate (0.04mol) and 3.17g of ammonium bicarbonate (0.04mol) in a ceramic mortar with a diameter of 160mm. At this time, the ratio of zinc sulfate heptahydrate and ammonium bicarbonate is 1:1. Without dispersion medium;

[0042] 2. Manually grind the solid mixture for 30 minutes;

[0043] 3. After the reaction, transfer the mixture in the ceramic mortar to a 50mL centrifuge bottle, add 10mL deionized water, stir the suspension with a glass rod for 3min, then centrifuge the suspension, filter, and continue to add deionized water , repeat the steps of washing and centrifugation 3 times, to remove unreacted complete reactant (zinc sulfate heptahydrate and ammonium bicarbonate) and ammonium sulfate;

[0044] 4. Dry the centrifuged solid at 60°C for 0.5h to obtain the precursor basic zinc carbonate;

[0045] 5. Put the precursor in a muffle furnace for calcination, the calcination temperature is 300° C., and the calcination time is 1 h...

Embodiment 2

[0049] 1. Weigh 5.76g zinc sulfate heptahydrate (0.02mol) and 3.17g ammonium bicarbonate (0.04mol) in a ceramic mortar with a diameter of 160mm. At this time, the ratio of zinc sulfate heptahydrate and ammonium bicarbonate is 1:2. Add the dispersion medium, the dispersion medium is 5mL ultrapure water;

[0050] 2. Manually grind the solid mixture for 60 minutes;

[0051] 3. After the reaction, transfer the mixture in the ceramic mortar to a 50mL centrifuge bottle, add 20mL of deionized water, stir the suspension with a glass rod for 4min, then centrifuge the suspension, filter, and continue to add deionized water , repeat the steps of washing and centrifugation 4 times, to remove unreacted complete reactant (zinc sulfate heptahydrate and ammonium bicarbonate) and ammonium sulfate;

[0052] 4. Dry the centrifuged solid at 70°C for 1 hour to obtain the precursor basic zinc carbonate;

[0053] 5. Put the precursor in a muffle furnace for calcination. The calcination temperature...

Embodiment 3

[0056] 1. Weigh 3.75g of zinc sulfate heptahydrate (0.013mol) and 3.17g of ammonium bicarbonate (0.04mol) in a ceramic mortar with a diameter of 160mm. At this time, the ratio of zinc sulfate heptahydrate and ammonium bicarbonate is 1:3. Add the dispersion medium, the dispersion medium is 5mL absolute ethanol;

[0057] 2. Manually grind the solid mixture for 90 minutes;

[0058] 3. After the reaction, transfer the mixture in the ceramic mortar to a 50mL centrifuge bottle, add 30mL deionized water, stir the suspension with a glass rod for 5min, then centrifuge the suspension, filter, and continue to add deionized water , repeat the steps of washing and centrifugation 5 times, to remove unreacted complete reactant (zinc sulfate heptahydrate and ammonium bicarbonate) and ammonium sulfate;

[0059] 4. Dry the centrifuged solid at 80°C for 2 hours to obtain the precursor basic zinc carbonate;

[0060] 5. Put the precursor in a muffle furnace for calcination. The calcination tempe...

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Abstract

The invention discloses a method for preparing multi-morphology nano zinc oxide by a solid phase method. The method comprises the following steps: (1) weighing zinc sulfate heptahydrate and ammonium bicarbonate into a ceramic mortar; (2) manually grinding the solid mixture; (3) after the reaction is finished, transferring the mixture in the ceramic mortar into a 50 mL centrifuge tube, adding 10 mL-30 mL of deionized water, stirring the turbid liquid for 3 min-5 min by using a glass rod, centrifuging the turbid liquid, filtering, continuously adding deionized water, and repeating the steps of washing and centrifuging for 3-5 times; (4) drying the centrifuged solid; (5) putting a precursor into a muffle furnace, and calcining; and (6) filling the calcined powder into a sample bag. The solid-phase method in the preparation method of zinc oxide is simple in process condition, low in cost, low in requirement on equipment, green and environment-friendly, high in zinc oxide yield, continuousand adjustable in operation procedure and easy to control the experimental process, so that industrial production is easy.

Description

technical field [0001] The invention relates to a preparation method of zinc oxide, in particular to a method for preparing multi-morphology nanometer zinc oxide by a solid phase method. Background technique [0002] Zinc oxide is an excellent direct band gap oxide semiconductor material with high thermal and chemical stability. It has a large energy band gap and exciton binding energy, high transparency, excellent room temperature luminescence performance and ultraviolet light and blue-green light emission capabilities, and is widely used in gas sensors, surface acoustic wave devices and light emitters. [0003] The preparation methods of nano zinc oxide mainly include chemical method and physical method. Chemical method is a method to nucleate atoms (or molecules) and grow them into nanoparticles by controlling the reaction conditions [Cui Lili, Fan Huili, Xiao Junping, etc. Research progress on surface modification of nanomaterials, Materials Herald, 2006, 20(S1): 5 -7]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82Y30/00B82Y40/00
CPCC01G9/02B82Y30/00B82Y40/00C01P2002/72C01P2004/03C01P2004/16C01P2004/30C01P2004/64C01P2004/32C01P2004/10
Inventor 吴月苗拯宁夏义文
Owner 淮南前景新材料有限公司
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