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Method for preparing lead tungstate nano-powder

A nano-powder, lead tungstate technology, applied in nanotechnology, chemical instruments and methods, tungsten compounds, etc., can solve the problems of large particle size, low specific surface area, waste of raw materials, etc., and achieve simple preparation method and post-processing Simple, Controllable Prepared Effects

Inactive Publication Date: 2012-11-14
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the problems of waste of raw materials, environmental pollution, large particle size, low specific surface area and uncontrollable size in the preparation process of lead tungstate powder materials at present, and provides a new reaction product self-emulsification precipitation method preparation The method of lead tungstate nanopowder expands the application of lead tungstate in the fields of luminescence, catalysis and radiation resistance

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  • Method for preparing lead tungstate nano-powder

Examples

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Effect test

Embodiment 1

[0033] (1) Under room temperature conditions, prepare respectively 0.02mol / L sodium stearate aqueous solution A and 0.1mol / L lead nitrate aqueous solution B (zirconium nitrate containing 1000ppm); 100mlA and 10mlB are mixed (the ratio of the amount of substance is Fatty acid sodium salt: soluble lead salt = 2: 1); after standing, filter and wash to obtain a precipitate of 0.001molC;

[0034] (2) Dissolve 0.001mol C in 100ml xylene to form a transparent emulsion D at a temperature of 90°C and a stirring speed of 5000r / min;

[0035] (3) Prepare 0.1mol / L tungstate aqueous solution; under the conditions of temperature 70°C and 5000r / min stirring speed, add 10ml of tungstate aqueous solution to D to form transparent / translucent emulsion E; The size adopts nanometer particle size analyzer (U.S., Malvern), and the size of nanoparticle is 14nm~20nm ( figure 1 );

[0036] (4) Cool to room temperature after the reaction, let it stand, wash the precipitate with ethanol and deionized wa...

Embodiment 2

[0038] (1) Under room temperature conditions, prepare 0.5mol / L sodium octanoate aqueous solution A and 1mol / L lead nitrate aqueous solution B respectively; 100mlA and 25mlB are mixed; After standing, filter and wash to obtain precipitate 0.025molC;

[0039] (2) Dissolve 0.025mol C in 100ml n-octane under the conditions of temperature 70°C and stirring speed 1000r / min to form transparent emulsion D;

[0040] (3) Prepare 0.125mol / L sodium tungstate aqueous solution; under the conditions of temperature 70°C and 1000r / min stirring speed, add 80ml of tungstate aqueous solution to D to form transparent / translucent emulsion E; latex particles The size adopts nanometer particle size analyzer (U.S., Malvern), and the size of nanoparticle is 85~95nm ( figure 2 );

[0041] (4) Cool to room temperature after the reaction, let it stand, wash the precipitate with ethanol and deionized water in turn, then dry at 100°C, and finally calcinate at 700°C in a muffle furnace for 4 hours to obtai...

Embodiment 3

[0043] (1) At room temperature, prepare 0.1mol / L sodium dodecylsulfonate aqueous solution A and 0.1mol / L lead nitrate aqueous solution B (containing 10ppm yttrium nitrate) respectively; mix 100mlA and 50mlB; filter after standing , washing to obtain a precipitate of 0.01molC;

[0044](2) Dissolve 0.01mol C in 100ml kerosene at a temperature of 60°C and a stirring speed of 3000r / min to form a transparent emulsion D;

[0045] (3) Prepare 0.25mol / L tungstate aqueous solution; under the conditions of temperature 70°C and 5000r / min stirring speed, add 40ml of tungstate aqueous solution dropwise to D to form translucent emulsion E; the size of latex particles adopts Nanoparticle size analyzer (USA, Malvern), the size of nanoparticles is 44 ~ 57nm ( image 3 );

[0046] (4) After the reaction is finished, cool to room temperature, let it stand, and wash the precipitate with ethanol and deionized water in turn, then dry it at 100°C, and finally calcinate it in a muffle furnace at 50...

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Abstract

The invention relates to a method for preparing a lead tungstate nano-powder by using a novel reactant self-emulsifying precipitation method. The method includes mixing a sodium aliphatate brine solution A and a soluble lead salt solution B (containing a trace amount of rare metal irons) according to a certain ratio of amount of substance, and subjecting the mixture to standing, filtering and washing to obtain a precipitate C; dissolving a certain amount of the C into a hot organic solvent to form a transparent emulsion D; dropwise adding a certain amount of a tungstic acid brine solution into the D to form an emulsion E; and cooling the emulsion E to the room temperature and subjecting the emulsion E to standing, precipitating, washing and drying, and calcining the emulsion E in a muffle furnace for 4 hours to obtain the lead tungstate nano-powder. According to the method, the prepared lead tungstate nano-powder reaches a nanoscale, the particle size of the lead tungstate nano-powder is 10-100nm, the morphology is regular, the distribution is narrow, the particle size of particles can be controlled by changing salinity of water phases, the operation is simple and convenient, the requirement on devices is low, and the method is applicable to scale production.

Description

technical field [0001] The invention relates to a preparation method of lead tungstate nano powder, which belongs to the field of nano material preparation. Background technique [0002] Lead tungstate is a very important inorganic material, which has broad application prospects in photoluminescence, microwave, scintillator, photocatalyst, etc. Compared with other inorganic tungstate crystals, lead tungstate has the advantages of high density, short irradiation length, fast attenuation, and strong anti-irradiation ability. Therefore, CERN uses lead tungstate crystals as scintillation crystals for the construction of high-resolution electromagnetic calorimeters on the Large Hadron Collider. Lead tungstate scintillation crystals, photomultiplier tubes, avalanche photodiodes, and silicon photodiodes compose detector components, which can be used in high-energy physics, nuclear physics, nuclear medical imaging, and industrial CT. Although various doping modifications of lead t...

Claims

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Application Information

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IPC IPC(8): C01G41/00B82Y40/00
Inventor 刘必前何敏杨海军吴杰李兰
Owner INST OF CHEM CHINESE ACAD OF SCI
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