Method for preparing phosphosilicate based glass

A phosphosilicate-based and silicic acid-based technology, which is applied in the field of preparation of phosphosilicate-based glass, can solve the problems of slow degradation rate, narrow component range, high reaction temperature, etc., and achieve good biocompatibility and small cytotoxicity , the effect of low reaction temperature

Active Publication Date: 2010-12-22
华魁科技泰州有限公司
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AI Technical Summary

Problems solved by technology

But this kind of bioglass has certain problems, such as the degradation rate is very slow, and it usually takes 1-2 years for complete degradation
The synthesis method used in this kind of bioglass-melt-extraction-cooling reaction temperature is too high to form porous materials, and it is difficult to achieve a high degree of compounding with organic materials to expand functions. Therefore, it is necessary to study new biomaterials and their preparation methods.
[0005] The introduction of phosphorus can usually increase the degradation rate of glass, but the range of biologically active components in phosphosilicate-based glasses prepared by traditional methods is relatively narrow, usually limited to low phosphorus content, which limits the improvement of glass degradation rate
When using the sol-gel method to prepare phosphosilicate-based glasses, it is usually found that the common precursors of phosphorus (such as phosphoric acid, triethyl phosphate, etc.) and the common precursors of calcium (such as calcium nitrate) have poor compatibility, which is easy to cause phase separation
In order to achieve effective mixing of phosphorus and calcium precursors, people sometimes have to choose a more toxic solvent (such as ethylene glycol) and reduce the concentration of the precursor, which will consume a lot of energy and time in the process of solvent removal , so that its practical operability is greatly reduced

Method used

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  • Method for preparing phosphosilicate based glass

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1: Preparation of phosphosilicate-based glass

[0026] According to the P in the phosphosilicate-based glass sample prepared in Table 1 2 o 5 , SiO 2 and CaO molar percentage content, the corresponding content of the precursor (phytic acid, ethyl orthosilicate and calcium nitrate tetrahydrate) is prepared into a gel precursor solution (calcium nitrate tetrahydrate is replaced by calcium chloride or calcium nitrate does not affect the results). First, take the precursor phytic acid in a 10ml sample bottle, and then add tetraethyl orthosilicate (TEOS), ethanol and water in sequence (the volume ratio is about 1:1, and the amount added should be enough to dissolve the aforementioned precursor), Stir for 30min, add Ca(NO 3 ) 2 4H 2O (or calcium chloride, or calcium nitrate), to obtain the gel precursor sol solution. Place the prepared gel precursor sol solution at room temperature until it gels (usually takes 2-10 days, depending on the ratio between the precu...

Embodiment 2

[0031] Embodiment 2: biological activity test

[0032] The phosphosilicate-based glass sample 2 (P 2 o 5 -24.4%, SiO 2 -40.6%, CaO-35.0%) soaked in simulated body fluid (SBF in Table 2) (37.0±0.5°C) for 14 days, a layer of dense and uniform hydroxyapatite formed on the surface of the sample. The microscopic morphology before and after soaking is as follows: Figure 1a and Figure 1b shown. The X-ray diffraction patterns before and after soaking are as follows: figure 2 shown.

[0033] Table 2: Ion concentrations in plasma (human body) and simulated human body fluid

[0034]

Embodiment 3

[0035] Embodiment 3: biological activity test

[0036] The bioactive phosphosilicate-based glass sample 3 (P 2 o 5 -16.6%, SiO 2 -18.4%, CaO-65.0%) soaked in simulated body fluid (SBF in Table 2) (37.0±0.5°C) for 14 days, a layer of dense and uniform hydroxyapatite formed on the surface of the sample. The microscopic morphology before and after soaking is as follows: Figure 3a and Figure 3b shown. The X-ray diffraction patterns before and after soaking are as follows: Figure 4 shown. and figure 2 It can be seen from the comparison of the X-ray diffraction pattern that the hydroxyapatite formation rate of sample 3 is faster than that of sample 2.

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Abstract

The invention belongs to the field of materials, and in particular relates to a method for preparing phosphosilicate based glass. The method takes water, ethanol or mixture of ethanol and water as solvent, and comprises the following steps: phytic acid, ethyl orthosilicate or calcium chloride are mixed to prepare gel precursor sol solution, and gel precursor sol solution is placed until becoming sol; the sol is aged at 60 DEG C, and is baked in an oven to ensure that the solvent is completely volatilized, and is cooled to room temperature; the temperature rises from the room temperature to the temperature of between 300 and 400 DEG C; and the dry gel is sintered at constant temperature of between 300 and 400 DEG C for at least 10 minutes, and is naturally cooled so as to obtain the phosphosilicate based glass. Compared with the conventional phosphorous precursor, the phytic acid serving as the precursor of phosphorous has smaller toxicity, so the biocompatibility of the material is improved, and the phosphosilicate based glass can be prepared in the conditions of low temperature, low toxicity and low cost, and the method can successfully prepare in a larger component range the phosphosilicate based glass with biodegradation speed which can be regulated in a wider range.

Description

technical field [0001] The invention belongs to the field of materials, in particular to a preparation method of phosphosilicate-based glass. Background technique [0002] With the increase of human life expectancy, artificial implant materials are facing new challenges. The life expectancy of more and more patients exceeds the designed service life of artificial implants, and they have to bear the pain of secondary surgery to replace implants. Therefore, it is necessary to design bioactive and biodegradable materials. [0003] In the early 1970s, Professor L.L. Hench of the University of Florida in the United States invented bioactive glass and applied it to the field of biomedicine for the first time, thus creating a new field of research on biomedical materials-bioactive glass and bioactive glass ceramics. As a biomedical material, this kind of material has incomparable advantages over metals, polymer materials and biologically inert materials, and can form a direct chem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C3/04
Inventor 邱东李爱玲
Owner 华魁科技泰州有限公司
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