CN103588187A - Preparation method of nano bioactive material - Google Patents
Preparation method of nano bioactive material Download PDFInfo
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- CN103588187A CN103588187A CN201310566640.4A CN201310566640A CN103588187A CN 103588187 A CN103588187 A CN 103588187A CN 201310566640 A CN201310566640 A CN 201310566640A CN 103588187 A CN103588187 A CN 103588187A
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Abstract
The invention discloses a preparation method of a nano bioactive material. The preparation method comprises the following steps: (1), weighing and adding a certain amount of Ca(OH)2 into 500 mL distilled water, stirring and blending uniformly; (2) dripping 200 mL phosphoric acid aqueous solution whose C(H3PO4) is equal to 0.3 mol/L into a calcium hydroxide/water suspension stirred at a high speed; (3) stirring for 5-15 h at a constant temperature after the dripping is finished, and aging for 10-24 h when the temperature is reduced to a room temperature; (4) filtering a white gelatinous precipitate and washing to remove residual impurities; and (5), performing freeze-drying for 24-72 h in a freeze dryer at the temperature of subzero 50 DEG C. The whole preparation process is simple, prepared nano-hydroxyapatite prepared with the process is uniform in particle size, good in histocompatibility, nontoxic and high in biological adhesion, has no immunogenicity, can serve as a medicine carrier, and can be also suitable for biomimetic materials of dentin and enamel.
Description
Technical field
The invention belongs to technical field of chemical material preparation, be specifically related to a kind of preparation method of nano bio-active material.
Background technology
Nano material and organism have close relationship dimensionally, and for example, the dimension of the ribonucleoprotein matter complex body of one of formation vital principle is between 15-20nm, and in organism, the size of various viruses is also in nanoscale scope.The birth of nanotechnology makes the ability of mankind's nature remodeling directly extend to molecule and atomic level, and making the mankind handle single atom according to the will of oneself becomes possibility.
Hydroxyapatite be animal and human's body bone want inorganic mineral composition, there is good biological activity and biocompatibility.When the size of hydroxyapatite reaches nano level, will reveal a series of special performance, as there is higher degraded and absorbability.Research shows: ultra-fine hydroapatite particles is inhibited to the growth of multiple cancer cells, and on normal cell without impact.
Nanometer hydroxyapatite as the distinguishing feature of biomaterial is, aspect composition, crystalline size and degree of crystallinity all with natural bone in osteolith very approaching, therefore there is extraordinary osteoinductive, in various bone reparing biological materials, be widely used.
At present, the preparation method of nanometer hydroxyapatite has many kinds, conventionally can be divided into wet method and dry method.Wet method comprises the precipitator method, hydrothermal method, sol-gel method, ultrasonic synthesis and microemulsion method etc., and dry method is solid state reaction etc.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method of nanometer hydroxyapatite is provided, the particle diameter of nanometer hydroxyapatite prepared by the method evenly and good dispersity.
Above-mentioned purpose of the present invention is achieved by the following scheme:
A preparation method for nano bio-active material, comprises the following steps:
1), take a certain amount of Ca (OH) 2 and join in 500mL distilled water, by agitator violent stirring, make it to mix until Ca (OH) 2 is more fine particle at distilled water distributes, form 0.1～0.3mol/L liming suspension;
2), set in the situation of reaction system n (Ca): n (P) >1.67, with constant flow pump, the phosphate aqueous solution of 200mLC (H3PO4)=0.3mol/L is splashed into the speed of 1mL/min in the 500mL calcium hydroxide/aqueous suspension of C Ca (OH) 2=0.25mol/L of high-speed stirring, whole reaction system constant temperature is at 50～55 ℃;
3), until step 2) all dropwise after again constant temperature stir 5～15h, the temperature of reaction solution is down to room temperature ageing 10～24h;
4), will after the gluey sedimentation and filtration of white, with deionized water wash, remove residual soluble impurity 3 times;
5), filter after in the freeze drier of-50 ℃ freeze-drying 24～72h, obtain white nanometer hydroxyapatite powder.
Further, above-mentioned steps 2) stirring velocity be 2000～3000r/min.
Compared with prior art, the beneficial effect that the present invention has is:
The whole preparation process of the present invention is simple and easy, the particle diameter of the nanometer hydroxyapatite of preparing by this technique is even, and histocompatibility is good, and nontoxic, non-immunogenicity, bioadhesive are strong, can be used as pharmaceutical carrier, also applicable to dentine and adamantine biomimetic material.
Embodiment
A preparation method for nano bio-active material, comprises the following steps:
1), taking a certain amount of Ca (OH) 2 joins in 500mL distilled water, by agitator violent stirring (stir speed (S.S.) is 2000r/min), make it to mix until Ca (OH) 2 is more fine particle distribution at distilled water, form 0.2mol/L liming suspension;
2), set in the situation of reaction system n (Ca): n (P) >1.67, with constant flow pump, the phosphate aqueous solution of 200mLC (H3PO4)=0.3mol/L be take to the speed of 1mL/min and splash in the 500mL calcium hydroxide/aqueous suspension of C Ca (OH) 2=0.25mol/L of high-speed stirring (stir speed (S.S.) is 2000r/min), whole reaction system constant temperature is at 50～55 ℃;
3), until step 2) all dropwise after again constant temperature stir (stir speed (S.S.) is 2000r/min) 10h, the temperature of reaction solution is down to room temperature ageing 10h;
4), will after the gluey sedimentation and filtration of white, with deionized water wash, remove residual soluble impurity 3 times;
5), filter after in the freeze drier of-50 ℃ freeze-drying 48h, obtain white nanometer hydroxyapatite powder.
Performance test: with X-ray diffractometer (XRD), material is carried out to phase and crystallinity analysis, carry out material grains pattern and size observation analysis with transmission electron microscope (TEM), carry out the chemical composition analysis of material with fourier-transform infrared instrument (IR).With liquid displacement technique, measure true density.
Result demonstration, each diffraction peak of the nanometer hydroxyapatite of preparation has not had overlapping phenomenon, and it is comparatively sharp-pointed that diffraction peak becomes, and peak shape is stronger, does not also have the diffraction peak of other impurity to occur.
Applicant's statement, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thereby the new numerical range producing, also be one of record scope of the present invention, the application, for making specification sheets simple and clear, is no longer enumerated these numerical ranges.
Claims (2)
1. a preparation method for nano bio-active material, is characterized in that, comprises the following steps:
1), take a certain amount of Ca (OH)
2join in 500mL distilled water, the speed stirring with agitator with 2000r/min makes it to mix, until Ca (OH)
2at distilled water, be more fine particle and distribute, form 0.1～0.3mol/L liming suspension;
2), set in the situation of reaction system n (Ca): n (P) >1.67, with constant flow pump by 200mLC (H
3pO
4the phosphate aqueous solution of)=0.3mol/L splashes into the C Ca (OH) of high-speed stirring with the speed of 1mL/min
2in 500mL calcium hydroxide/aqueous suspension of=0.25mol/L, whole reaction system constant temperature is at 50～55 ℃;
3), until step 2) all dropwise after again constant temperature stir 5～15h, the temperature of reaction solution is down to room temperature ageing 10～24h;
4), will after the gluey sedimentation and filtration of white, with deionized water wash, remove residual soluble impurity 3 times;
5), filter after in the freeze drier of-50 ℃ freeze-drying 24～72h, obtain white nanometer hydroxyapatite powder.
2. the preparation method of a kind of nano bio-active material as claimed in claim 1, is characterized in that: stirring velocity described step 2) is 2000～3000r/min.
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| CN201310566640.4A CN103588187A (en) | 2013-11-14 | 2013-11-14 | Preparation method of nano bioactive material |
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| CN201310566640.4A CN103588187A (en) | 2013-11-14 | 2013-11-14 | Preparation method of nano bioactive material |
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| CN103588187A true CN103588187A (en) | 2014-02-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104587982A (en) * | 2015-01-16 | 2015-05-06 | 兰州大学 | Material capable of enriching and separating uranium in water solution and preparation method of material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153059A (en) * | 2011-04-13 | 2011-08-17 | 上海师范大学 | Method for preparing monodisperse hydroxyapatite by taking blue algae as template |
| CN102861356A (en) * | 2012-10-19 | 2013-01-09 | 南京信息工程大学 | Bone repairing material and preparation method thereof |
| CN103112837A (en) * | 2013-03-18 | 2013-05-22 | 厦门大学 | Preparation method of nano-hydroxyapatite |
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2013
- 2013-11-14 CN CN201310566640.4A patent/CN103588187A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153059A (en) * | 2011-04-13 | 2011-08-17 | 上海师范大学 | Method for preparing monodisperse hydroxyapatite by taking blue algae as template |
| CN102861356A (en) * | 2012-10-19 | 2013-01-09 | 南京信息工程大学 | Bone repairing material and preparation method thereof |
| CN103112837A (en) * | 2013-03-18 | 2013-05-22 | 厦门大学 | Preparation method of nano-hydroxyapatite |
Non-Patent Citations (1)
| Title |
|---|
| 王艳莉 等: "氢氧化钙-磷酸体系在沉淀法合成羟基磷灰石过程中原料粒度的影响", 《硅酸盐学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104587982A (en) * | 2015-01-16 | 2015-05-06 | 兰州大学 | Material capable of enriching and separating uranium in water solution and preparation method of material |
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