Preparation method of hydroxyapatite containing Sn(II)

A hydroxyapatite and group technology, which is applied in the field of preparation of Sn-containing hydroxyapatite, can solve the problems of high temperature, do not contain biological active materials such as hydroxyapatite, increase production cost, etc., and achieve uniform particle size and phase. high purity effect

Active Publication Date: 2014-12-10
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] At present, there are literature reports [Procter & Gamble Company. Advanced stannous - sodium fluoride toothpaste [J]. Oral Care Products Industry, 2012 (1): 23-31. ] Oral care products containing stannous, but such oral care products only have antibacterial and tooth-fixing functions, and do not contain bioactive materials such as hydroxyapatite
At present, the preparation of hydroxyapatite materials containing other elements in the literature requires heat treatment, which requires high temperature and consumes energy, thereby increasing the production cost

Method used

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  • Preparation method of hydroxyapatite containing Sn(II)
  • Preparation method of hydroxyapatite containing Sn(II)
  • Preparation method of hydroxyapatite containing Sn(II)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) First, dissolve calcium chloride and stannous chloride in hydrochloric acid solution to obtain solution A, and Sn in solution A 2+ and Ca 2+ The molar ratio Sn / (Ca+Sn)=0.01;

[0032] 2) Second, will contain H 3 PO 4 The phosphoric acid solution of the group is added to solution A according to the molar ratio of (Ca+Sn):P=10:6, and then NaOH solution is added to adjust the solution to be alkaline to obtain a mixed solution;

[0033] 3) Transfer the mixed solution to an oven for reaction, control the reaction temperature at 60°C, and react for 48 hours;

[0034] 4) Filter the reacted solution under reduced pressure, rinse with alkaline solution, and finally rinse the filter cake with distilled water until neutral;

[0035] 5) Move the filter cake to an oven to dry and then prepare the desired powder.

[0036] The XRD diffraction pattern of gained powder is as figure 1 As shown, the phase shown in the figure is hydroxyapatite phase, the diffraction peak has a cert...

Embodiment 2

[0038] 1) First, dissolve calcium nitrate and stannous nitrate in nitric acid solution to obtain solution A. In solution A, Sn 2+ and Ca 2+ The molar ratio Sn / (Ca+Sn)=0.1;

[0039] 2) Second, will contain H 2 PO 4 - The potassium dihydrogen phosphate of the group is added to the solution A according to the molar ratio of (Ca+Sn):P=10:6, and then the KOH solution is added to adjust the solution to be alkaline to obtain a mixed solution;

[0040] 3) Transfer the mixed solution to an oven for reaction, control the reaction temperature at 80°C, and react for 30 hours;

[0041] 4) Filter the reacted solution under reduced pressure, rinse with alkaline solution, and finally rinse the filter cake with distilled water until neutral;

[0042] 5) Move the filter cake to an oven to dry and then prepare the desired powder.

Embodiment 3

[0044] 1) First, dissolve calcium chloride and stannous sulfate in hydrochloric acid solution to obtain solution A, and Sn in solution A 2+ and Ca 2+ The molar ratio Sn / (Ca+Sn)=0.05;

[0045] 2) Second, will contain H 2 PO 4 - The sodium dihydrogen phosphate solution of the group is added to solution A according to the molar ratio of (Ca+Sn):P=10:6, and then NH 3 ·H 2 The O solution adjusts the solution to be alkaline to obtain a mixed solution;

[0046]3) Transfer the mixed solution to an oven for reaction, control the reaction temperature at 70°C, and react for 36 hours;

[0047] 4) Filter the reacted solution under reduced pressure, rinse with alkaline solution, and finally rinse the filter cake with distilled water until neutral;

[0048] 5) Move the filter cake to an oven to dry and then prepare the desired powder.

[0049] Its SEM picture is as image 3 As shown, the corresponding energy spectrum analysis shows that the molar ratio of (Ca+Sn) / P is 1.6678, which ...

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Abstract

The invention relates to a preparation method of hydroxyapatite containing Sn(II). The preparation method comprises the following steps of: firstly adding a solution containing Ca<2+> and Sn<2+> into a solution containing H3PO4 / H2PO<4-> / HPO4<2-> / PO4<3-> in mol ratio that (Ca+Sn) / P is equal to 10 / 6, adjusting a solution system to be alkaline, reacting for 12-48 hours at the temperature of 60-100 DEG C, and then washing to a pure phase; and carrying out suction filtering to obtain powder. A hydroxyapatite phase is observed by carrying out XRD (X-ray diffraction) on the prepared powder, particle diameter is observed to be in uniform distribution by utilizing an SEM (scanning electron microscope), granules are spherical, granular size is about 20nm, Ca<2+> is released in a dissolution process and Sn<2+> is also released, Ca<2+> can slow down a dissolution reaction on the surface of teeth, and Sn<2+> can inhibit activity of anaerobic bacteria in a mouth cavity; and hydroxyapatite powder can serve as a grinding material, has hardness similar to that of teeth, can effectively reduce tooth abrasion in a tooth brushing process and has a good characteristic of protecting mouth health.

Description

technical field [0001] The invention relates to a method for preparing hydroxyapatite powder, in particular to a method for preparing hydroxyapatite containing Sn(II). Background technique [0002] In recent years, the incidence of oral diseases in children has been increasing year by year. With the accelerated pace of life and the improvement of quality of life, the probability of oral diseases is also increasing. The incidence of oral diseases represented by dental caries is increasing year by year. Even adult rates of dental caries are rising. The existing oral care products with antibacterial function mainly rely on the addition of antibiotics to achieve antibacterial purposes, but long-term use of antibiotics will cause bacteria to develop drug resistance and have certain toxicity to users. Therefore, it is meaningful to prepare oral care product additives that do not contain antibiotics and have antibacterial functions. [0003] Hydroxyapatite is the main component o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45
Inventor 殷海荣吴阳刘盼郭宏伟扈东玖杜胜蔡小正郭变红
Owner SHAANXI UNIV OF SCI & TECH
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