A kind of preparation method of calcium fluoride microsphere

A technology of calcium fluoride and microspheres, applied in the direction of calcium/strontium/barium fluoride, calcium/strontium/barium halide, etc., can solve the problems of high production cost and harsh reaction conditions, and achieve convenient operation and mild reaction conditions , The effect of simple preparation process equipment

Inactive Publication Date: 2017-07-28
SHANDONG JIANZHU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation methods of nano-calcium fluoride mainly include direct precipitation method, microemulsion method and hydrothermal method. Although these methods can synthesize nano-calcium fluoride microspheres, the reaction conditions are relatively harsh and the production cost is high.

Method used

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  • A kind of preparation method of calcium fluoride microsphere
  • A kind of preparation method of calcium fluoride microsphere
  • A kind of preparation method of calcium fluoride microsphere

Examples

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Effect test

Embodiment 1

[0030] 1 g of commercially available octacalcium phosphate (Ca 8 (HPO 4 ) 2 (PO 4 )·5H 2 O) powder, put into 500mL distilled water, stir with magnetic stirrer, with the phosphoric acid (H of 0.01mol / L NaOH solution and 0.01mol / L 3 PO 4 ) to carry out acid-base titration to keep the pH value of the solution at 5.2, the temperature is 20°C, stir with a magnetic stirrer for 1 hour, and add 0.5mol / L of NH 4 F solution 100mL, continue to stir for 24h. The suspension was filtered with distilled water, and when the pH value of the filtered solution was neutral, it was filtered twice with absolute ethanol, and dried in an environment of 40°C to obtain calcium fluoride (CaF 2 )Microspheres. figure 1 and figure 2 calcium fluoride (CaF 2 ) transmission electron microscope picture and XRD pattern, by figure 1 It can be seen that the product is a hollow microsphere with a diameter of 200nm to 800nm, the size of the microsphere is relatively uniform, the shape is consistent, and ...

Embodiment 2

[0032] 1 g of commercially available hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2) powder, put into 500mL distilled water, stir with a magnetic stirrer, use 0.01mol / L NaOH solution and 0.01mol / L phosphoric acid (H 3 PO 4 ) to carry out acid-base titration to keep the pH value of the solution at 5.5, the temperature is 20°C, stir with a magnetic stirrer for 1 hour, and add 0.5mol / L of NH 4 F solution 100mL, continue to stir for 24h. The suspension was filtered with distilled water, and when the pH value of the filtered solution was neutral, it was filtered twice with absolute ethanol, and dried in an environment of 40°C to obtain calcium fluoride (CaF 2 )Microspheres. image 3 and Figure 4 calcium fluoride (CaF 2 ) transmission electron microscope picture and XRD pattern, image 3 It can be seen that the product is a hollow microsphere with a diameter of 200nm to 800nm, the size of the microsphere is relatively uniform, the shape is consistent, and it is approximately spher...

Embodiment 3

[0034] Commercially available 1 g β-tricalcium phosphate (Ca 3 (PO 4 ) 2 ) powder, put into 500mL distilled water, stir with a magnetic stirrer, use 0.01mol / L NaOH solution and 0.01mol / L phosphoric acid (H 3 PO 4 ) to carry out acid-base titration to keep the pH value of the solution at 6.0, the temperature is 20°C, stir with a magnetic stirrer for 1 hour, and add 0.5mol / L of NH 4 F solution 100mL, continue to stir for 24h. The suspension was filtered with distilled water, and when the pH value of the filtered solution was neutral, it was filtered twice with absolute ethanol, and dried in an environment of 40°C to obtain calcium fluoride (CaF 2 )Microspheres. Figure 5 and Figure 6 calcium fluoride (CaF 2 ) transmission electron microscope picture and XRD pattern, Figure 5 It can be seen that the product is a hollow microsphere with a diameter of 200nm to 800nm, the size of the microsphere is relatively uniform, the shape is consistent, and it is approximately spheri...

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Abstract

The invention discloses a preparation method of calcium fluoride microspheres, which uses an acid-base titration method to keep the solution acidic, dissolves insoluble calcium and phosphorus salts to generate calcium ions, and adds soluble fluoride salt solutions to provide fluoride ions, thereby preparing fluoride Calcium (CaF 2 )Microspheres. The steps are to put insoluble calcium calcium phosphate into the weakly acidic solution maintained by acid-base titration, stir with a magnetic stirrer for 1 hour to form a suspension, add a certain amount of soluble fluorine salt solution, and stir with a magnetic stirrer 24 hours. The suspension was filtered successively with distilled water and absolute ethanol, and then dried at 40°C to obtain calcium fluoride (CaF 2 )Microspheres. The method has simple steps, mild conditions and is easy for industrial production.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to a preparation method of calcium fluoride microspheres. Background technique [0002] Scientific research has confirmed that the commonly used fluoride toothpaste or mouthwash can provide saliva with a low concentration of fluorine, and the use of fluoride toothpaste or fluoride mouthwash can prevent dental caries to a certain extent. However, because fluoride toothpaste or mouthwash exists in the oral cavity for a short time, the time for the oral cavity to contain effective fluorine is also very short. The best way is to have a source of fluorine element in the oral cavity that continuously releases small doses of fluorine element to form an environment with low concentration of fluoride ions, which can prevent dental diseases such as dental caries, and will not harm the human body due to excessive fluoride ion concentration healthy. [0003] Calcium Fluoride (CaF...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F11/22
Inventor 岳雪涛徐丽娜张丰庆李静井敏房永广隋玉武田清波孙德明孙康宁
Owner SHANDONG JIANZHU UNIV
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