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Preparation method of CaWO4 hollow spheres

A hollow ball and air technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of affecting material properties, cumbersome operation process, inconvenient product cleaning, etc., and achieves low reaction temperature, simple raw materials, and easy operation. Effect

Inactive Publication Date: 2012-10-03
无锡润鹏复合新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires the action of a surfactant to disperse the particles and generate calcium tungstate with a hollow spherical structure. On the one hand, it makes the operation process cumbersome and increases the cost; performance

Method used

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  • Preparation method of CaWO4 hollow spheres
  • Preparation method of CaWO4 hollow spheres
  • Preparation method of CaWO4 hollow spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under magnetic stirring, 0.2mol / L, 25ml Na 2 WO 4 and 0.2mol / L, 25mlCaCl 2 Mix, adjust the pH value of the mixed solution to 9 with the NaOH of 0.2mol / L and the HCl of 0.2mol / L, stir for 10min, after mixing evenly, transfer the mixed solution into an autoclave with a polytetrafluoroethylene liner. React in a constant temperature box at 160°C for 24 hours, cool down to room temperature with the furnace, open the reaction kettle, decant the upper layer, wash thoroughly with distilled water and absolute ethanol in turn, and filter under reduced pressure at room temperature to obtain a white solid product. Dry at 80°C for 4 hours to obtain dispersed micron CaWO 4 hollow ball. attached figure 1 It is the X-ray diffraction pattern of the product obtained in this example, as can be seen from the figure, no impurity peak appears, indicating that the product is pure CaWO 4 . attached figure 2 It is the low-magnification SEM figure of the product obtained in this embodime...

Embodiment 2

[0030] Under magnetic stirring, 0.2mol / L, 25ml Na 2 WO 4 and 0.2mol / L, 25mlCaCl 2 Mix, adjust the pH value of the mixed solution to 7 with the NaOH of 0.2mol / L and the HCl of 0.2mol / L, stir 10min, after mixing evenly, transfer the mixed solution into an autoclave with a polytetrafluoroethylene liner, React in a constant temperature box at 160°C for 24 hours, cool down to room temperature with the furnace, open the reaction kettle, decant the upper layer, wash thoroughly with distilled water and absolute ethanol in turn, and filter under reduced pressure at room temperature to obtain a white solid product. Dry at 80°C for 4 hours to obtain dispersed calcium tungstate microspheres. As can be seen from the X-ray diffraction pattern of this embodiment, the resulting product CaWO 4 High purity, no other impurities. As can be seen from the SEM image of this embodiment, the CaWO generated under the experimental conditions 4 , the particle dispersibility is better, but the obtain...

Embodiment 3

[0032] Under magnetic stirring, 0.2mol / L, 25ml Na 2 WO 4 and 0.2mol / L, 25mlCaCl 2Mix, adjust the pH value of the mixed solution to 11 with the NaOH of 0.2mol / L and the HCl of 0.2mol / L, stir for 10min, after mixing evenly, transfer the mixed solution into an autoclave with a polytetrafluoroethylene liner. React in a constant temperature box at 160°C for 24 hours, cool down to room temperature with the furnace, open the reaction kettle, decant the upper layer, wash thoroughly with distilled water and absolute ethanol in turn, and filter under reduced pressure at room temperature to obtain a white solid product. Dry at 80°C for 4 hours to obtain dispersed calcium tungstate microspheres.

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Abstract

The invention discloses a method for preparing dispersed CaWO4 micrometer-sized hollow spheres. Sodium tungstate and calcium chloride are mixed, the pH value of the mixed solution is adjusted by hydrochloric acid and sodium hydroxide, the solution is uniformly mixed under the action of magnetic stirring, and then the mixed solution is subjected to hydrothermal reaction in an autoclave with a polytetrafluoroethylene liner, after furnace cooling, the product is washed, filtered and dried, and then calcium tungstate microspheres with the diameter of 3 microns to 5micros can be obtained. With the invention, dispersed calcium tungstate micrometer-sized hollow spheres can be synthetized at one step without adding any surfactant, the synthesis temperature is lower, and the method is simple, and is easy to operate.

Description

technical field [0001] The invention relates to the field of inorganic micron powder materials, in particular to a method for preparing dispersible calcium tungstate micron hollow spheres. Background technique [0002] Calcium tungstate (CaWO 4 ) is a typical self-activated luminescent material with stable physical and chemical properties. Calcium tungstate is a very effective luminescent material under X-ray, electron beam and ultraviolet excitation. As early as the late 19th century, people began to study CaWO 4 The study of crystal properties. Due to its unique optical properties, CaWO 4 It can be used as phosphor, radiation intensity scintillation counting material and laser host material. [0003] At present, the methods for preparing calcium tungstate microspheres include microemulsion thermal synthesis technology, chemical precipitation method and so on. Use microemulsion thermal synthesis technology as SUN etc., add surfactant hexadecyl tricresyl ammonium bromi...

Claims

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Application Information

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IPC IPC(8): C01G41/00
Inventor 李长生唐华季晓瑞范有志孙建荣钱周
Owner 无锡润鹏复合新材料有限公司
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