CN103541005B - A kind of preparation method of magnetic hydroxylapatite crystal whisker ball - Google Patents
A kind of preparation method of magnetic hydroxylapatite crystal whisker ball Download PDFInfo
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Abstract
The preparation method of a kind of magnetic hydroxylapatite crystal whisker ball of disclosure, the method is with soluble calcium salt, solubility microcosmic salt, the double-deck nano ferriferrous oxide magnetic fluid modified for raw material, carbamide is acidity-basicity regulator, prepares magnetic hydroxylapatite crystal whisker ball under 75 ~ 80 DEG C of water bath condition；Present invention process is simple, it is simple to operation, stable yield, products obtained therefrom function admirable, can be used for the fields such as target medicine carrier, biological engineering material。
Description
Technical field
The preparation method that the present invention relates to a kind of magnetic hydroxylapatite crystal whisker ball, belongs to target medicine carrier and biological engineering material field。
Background technology
Hydroxyapatite (Ca10(PO4)6(OH)2), it is called for short HA or HAP, there is good biocompatibility；Diameter is different from block magnetic material at several ferroso-ferric oxide to tens nanometers, show as superparamagnetism: in magnetic field, namely have relatively ferromagnetism, when not having magnetic field, magnetic quickly disappears, and there have zoopery to demonstrate nano ferriferrous oxide biocompatibility to be better, can excrete with body fluid metabolic。
At present, it is domestic that to prepare hydroxyapatite crystal whisker ball more rare, hydroxyapatite crystal whisker ball main manifestations becomes a kind of dephasign in hydroxyapatite crystal whisker preparation process, its productivity is non-normally low, hydroxyapatite crystal whisker ball not only productivity prepared by this patent is higher, and whisker ball center is with the magnetic core of a nano ferriferrous oxide, can magnetic control targeting。The raising of its productivity is primarily due to employ the nano ferriferrous oxide of double; two decorative layer as magnetic core, and its outer layer dressing agent is the template such as sorbitol, and this is conducive to the growth of whisker, and being more beneficial for whisker, to grow up to radioactivity along template spherical。Meanwhile, the nano ferriferrous oxide after double; two modifieds has good suspendability, and the growth for whisker provides reliable and stable growing space。
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of magnetic hydroxylapatite crystal whisker ball, specifically includes following steps:
(1) be in molar ratio 1:1:5 ~ 2.5:1:15 ratio by soluble calcium salt, solubility microcosmic salt, carbamide mixing, feed the mixture in distilled water in the ratio of 10 ~ 100g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 2 ~ 3, than the ratio for 1:1 ~ 1:10, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in double-deck modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 5 ~ 30 minutes；
(2) arranging bath temperature is 70 ~ 80 DEG C, isothermal reaction 10 ~ 36 hours, and question response terminates, and takes out product distilled water and cleans 3 ~ 8 times；
(3) product that step (3) obtains obtains whisker filter cake after sucking filtration, freeze-day with constant temperature 8 ~ 20 hours in 45 DEG C ~ 80 DEG C calorstats, or vacuum lyophilization 48h, cryogenic temperature-20 DEG C ~-40 DEG C, vacuum is 20pa, obtains magnetic hydroxylapatite crystal whisker ball。
Soluble calcium salt of the present invention is the solvable calcium salt being dissolved in water such as calcium nitrate, calcium chloride。
Solubility microcosmic salt of the present invention is water-soluble phosphate, hydrophosphate and the dihydric phosphates such as diammonium phosphate。
Double-deck modification nano ferriferrous oxide magnetic fluid of the present invention, concrete preparation method is as follows:
A, it is 1.9:1 ~ 2.1:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 5 ~ 50g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:2 ~ 1:6 of stearic acid and iron ion；Regulate bath temperature be 60 ~ 90 DEG C, then in mixed liquor add ammonia, the PH making solution is 8 ~ 10, react 20 ~ 40min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
C, it is dissolved in distilled water obtains outer layer dressing agent solution by ultrasonic for outer layer dressing agent, monolayer is modified nano ferriferrous oxide and adds in outer layer dressing agent solution, mol ratio 1:1 ~ the 6:1 of its ectomesoderm dressing agent and iron ion, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
Outer layer dressing agent of the present invention is the one in sorbitol, cetyl trimethylammonium bromide, Polyethylene Glycol。
The invention has the beneficial effects as follows:
(1) magnetic whisker ball preparation method reaction process of the present invention is simple, and stable yield is easy and simple to handle；
(2) productivity of the magnetic whisker ball that preparation method of the present invention prepares is high, and magnetic whisker ball has excellent magnetic characteristics, and shows superparamagnetism, even size distribution；
(3) biocompatibility stating the magnetic whisker ball that preparation method prepares of the present invention and activity are good, can be used for the association area such as target medicine carrier and biological engineering material。
Accompanying drawing explanation
Fig. 1: magnetic hydroxylapatite crystal whisker ball process chart；
Fig. 2: the inversion microphotograph of magnetic hydroxylapatite crystal whisker ball；
Fig. 3: the XRD figure spectrum of magnetic hydroxylapatite crystal whisker ball；
Fig. 4: the SEM photograph of magnetic hydroxylapatite crystal whisker ball；
Fig. 5: the EDS collection of illustrative plates of magnetic hydroxylapatite crystal whisker ball。
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but scope is not limited to described content。
Embodiment 1
Shown in the process chart of the preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment such as accompanying drawing 1, specifically include following steps:
The preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment, specifically includes following steps:
(1) be in molar ratio 1:1:5 ratio by four water-calcium nitrate, disodium-hydrogen, carbamide mixing, feed the mixture in distilled water in the ratio of 100g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 2.5, than the ratio for 1:1, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in bilayer modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 5 minutes；
(2) arranging bath temperature is 70 DEG C, and along with the carrying out of reaction, carbamide constantly decomposites amine, and amine is dissolved in and being risen by the pH value making solution, isothermal reaction 36 hours, and question response terminates, and takes out product distilled water and cleans 5 times；
(3) product that step (2) obtains obtains whisker filter cake after sucking filtration, and in 60 DEG C of calorstats, freeze-day with constant temperature 24 hours, obtain magnetic hydroxylapatite crystal whisker ball。
Double-deck modification nano ferriferrous oxide magnetic fluid described in the present embodiment, concrete preparation method is as follows:
A, it is 2:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 5g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:2 of stearic acid and iron ion；Regulate bath temperature be 60 DEG C, then in mixed liquor add ammonia, the PH making solution is 9, react 30min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of sorbitol weighed in the ratio of 0.5g/L, the mol ratio 1:1 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:4 is by above-mentioned monolayer modification nano ferriferrous oxide addition sorbitol solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
The magnetic hydroxylapatite crystal whisker ball that the present embodiment prepares, even size distribution, as described in Figure 2, prepared whisker ball mean radius is about 40 microns, as shown in Figure 4, surface is crystal whisker-shaped, contains ferrum according to the known center in whisker ball of Fig. 5, and the XRD of 3 can be concluded that with reference to the accompanying drawings, ferrum is to exist with the form of ferroso-ferric oxide, therefore, the magnetic hydroxylapatite crystal whisker ball that the present embodiment preparation prepares is core is nano ferriferrous oxide, and surface is the ball of hydroxyapatite crystal whisker。
Embodiment 2
The preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment, specifically includes following steps:
(1) be in molar ratio 1:1:5 ratio by four water-calcium nitrate, sodium phosphate, carbamide mixing, feed the mixture in distilled water in the ratio of 100g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 2, than the ratio for 1:1, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in bilayer modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 5 minutes；
(2) arranging bath temperature is 70 DEG C, and along with the carrying out of reaction, carbamide constantly decomposites amine, and amine is dissolved in and being risen by the PH making solution, isothermal reaction 36 hours, and question response terminates, and takes out product distilled water and cleans 3 times；
(3) product that step (2) obtains obtains whisker filter cake after sucking filtration, and in 45 DEG C of calorstats, freeze-day with constant temperature 20 hours, obtain magnetic hydroxylapatite crystal whisker ball。
Double-deck modification nano ferriferrous oxide magnetic fluid described in the present embodiment, concrete preparation method is as follows:
A, it is 2:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 5g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:2 of stearic acid and iron ion；Regulate bath temperature be 60 DEG C, then in mixed liquor add ammonia, the PH making solution is 8, react 40min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of sorbitol weighed in the ratio of 0.5g/L, the mol ratio 1:1 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:4 is by above-mentioned monolayer modification nano ferriferrous oxide addition sorbitol solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
The magnetic hydroxylapatite crystal whisker ball that this enforcement prepares, even size distribution, surface whisker is bar-shaped, whisker length is about 5 microns, the radius of ball is about 10 microns, it is possible to as a kind of good medicine carrying material, magnetic property shows as superparamagnetism, the magnetic hydroxylapatite crystal whisker ball that the present embodiment preparation prepares is core is nano ferriferrous oxide, and surface is the ball of hydroxyapatite crystal whisker。
Embodiment 3
The preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment, specifically includes following steps:
(1) be in molar ratio 1.5:1:12 ratio by calcium chloride, phosphoric acid one hydrogen amine, carbamide mixing, feed the mixture in distilled water in the ratio of 10g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 3, than the ratio for 1:4, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in bilayer modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 18 minutes；
(2) arranging bath temperature is 72 DEG C, and along with the carrying out of reaction, carbamide constantly decomposites amine, and amine is dissolved in and being risen by the PH making solution, isothermal reaction 16 hours, and question response terminates, and takes out product distilled water and cleans 4 times；
(3) product that step (2) obtains obtains whisker filter cake, vacuum lyophilization after sucking filtration, and wherein temperature is-40 DEG C, and vacuum is 20Pa, and drying time, 48h, obtained magnetic hydroxylapatite crystal whisker ball。
Double-deck modification nano ferriferrous oxide magnetic fluid described in the present embodiment, concrete preparation method is as follows:
A, it is 2:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 50g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:6 of stearic acid and iron ion；Regulate bath temperature be 90 DEG C, then in mixed liquor add ammonia, the PH making solution is 10, react 20min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of cetyl trimethylammonium bromide weighed in the ratio of 0.5g/L, the mol ratio 6:1 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:6 is by above-mentioned monolayer modification nano ferriferrous oxide addition cetyl trimethylammonium bromide solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
The magnetic hydroxylapatite crystal whisker ball that the present embodiment prepares, even size distribution, smooth surface no-sundries, whisker length is 100 nanometers, its average radius of a ball is about 250 nanometers, it is possible to as a kind of good medicine carrying material, magnetic property shows as superparamagnetism, the magnetic hydroxylapatite crystal whisker ball that the present embodiment preparation prepares is core is nano ferriferrous oxide, and surface is the ball of hydroxyapatite crystal whisker。
Embodiment 4
The preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment, specifically includes following steps:
(1) it is that the ratio of 2:1:8 is by calcium nitrate and sodium dihydrogen phosphate, carbamide mixing in molar ratio, feed the mixture in distilled water in the ratio of 30g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 2.5, than the ratio for 1:8, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in bilayer modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 20 minutes；
(2) arranging bath temperature is 74 DEG C, and along with the carrying out of reaction, carbamide constantly decomposites amine, and amine is dissolved in and being risen by the PH making solution, isothermal reaction 25 hours, and question response terminates, and takes out product distilled water and cleans 6 times；
(3) product that step (2) obtains obtains whisker filter cake, vacuum lyophilization after sucking filtration, and wherein temperature is-40 DEG C, and vacuum is 20Pa, and drying time, 48h, obtained magnetic hydroxylapatite crystal whisker ball。
Double-deck modification nano ferriferrous oxide magnetic fluid described in the present embodiment, concrete preparation method is as follows:
A, it is 2:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 20g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:3 of stearic acid and iron ion；Regulate bath temperature be 70 DEG C, then in mixed liquor add ammonia, the PH making solution is 9, react 30min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of Polyethylene Glycol weighed in the ratio of 0.5g/L, the mol ratio 1:2 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:5 is by above-mentioned monolayer modification nano ferriferrous oxide addition polyglycol solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
The magnetic hydroxylapatite crystal whisker ball that the present embodiment prepares, even size distribution, smooth surface no-sundries, whisker length is 10 microns, and its average radius of a ball is about 20 microns, and surface is nano bar-shape crystalline substance, can as a kind of good medicine carrying material, magnetic property shows as superparamagnetism, and the magnetic hydroxylapatite crystal whisker ball that the present embodiment preparation prepares is core is nano ferriferrous oxide, and surface is the ball of hydroxyapatite crystal whisker。
Embodiment 5
The preparation method of magnetic hydroxylapatite crystal whisker ball described in the present embodiment, specifically includes following steps:
(1) it is that the ratio of 2.5:1:15 is by calcium nitrate and sodium dihydrogen phosphate, carbamide mixing in molar ratio, feed the mixture in distilled water in the ratio of 60g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 3, than the ratio for 1:10, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in bilayer modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 30 minutes；
(2) arranging bath temperature is 80 DEG C, and along with the carrying out of reaction, carbamide constantly decomposites amine, and amine is dissolved in and being risen by the PH making solution, isothermal reaction 10 hours, and question response terminates, and takes out product distilled water and cleans 3 ~ 8 times；
(3) product that step (2) obtains obtains whisker filter cake after sucking filtration, freeze-day with constant temperature 8 hours in 80 DEG C of calorstats, or vacuum lyophilization, obtains magnetic hydroxylapatite crystal whisker ball。
Double-deck modification nano ferriferrous oxide magnetic fluid described in the present embodiment, concrete preparation method is as follows:
A, it is 2:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 40g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:4 of stearic acid and iron ion；Regulate bath temperature be 80 DEG C, then in mixed liquor add ammonia, the PH making solution is 9.5, react 35min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of sorbitol weighed in the ratio of 0.5g/L, the mol ratio 1:4 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:5.5 is by above-mentioned monolayer modification nano ferriferrous oxide addition sorbitol solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid。
The magnetic hydroxylapatite crystal whisker ball that the present embodiment prepares, even size distribution, smooth surface no-sundries, whisker length is 15 microns, and its average radius of a ball is about 30 microns, it is possible to as a kind of good medicine carrying material, magnetic property shows as superparamagnetism, its regularity is better, and the magnetic hydroxylapatite crystal whisker ball that the present embodiment preparation prepares is core is nano ferriferrous oxide, and surface is the ball of hydroxyapatite crystal whisker。
Claims (2)
1. the preparation method of a magnetic hydroxylapatite crystal whisker ball, it is characterised in that: comprise the steps:
(1) be in molar ratio 1:1:5 ~ 2.5:1:15 ratio by soluble calcium salt, solubility microcosmic salt, carbamide mixing, feed the mixture in distilled water in the ratio of 10 ~ 100g/L, treat that all medicines dissolve, the initial pH of solution is regulated with concentrated nitric acid, making pH value is 2 ~ 3, than the ratio for 1:1 ~ 1:10, bilayer is modified nano ferriferrous oxide magnetic fluid with mixed liquor volume in double-deck modification nano ferriferrous oxide magnetic fluid and join in mixed solution, ultrasonic disperse 5 ~ 30 minutes；
(2) arranging bath temperature is 70 ~ 80 DEG C, isothermal reaction 10 ~ 36 hours, and question response terminates, and takes out product distilled water and cleans 3 ~ 8 times；
(3) product that step (2) obtains obtains whisker filter cake after sucking filtration, obtains magnetic hydroxylapatite crystal whisker ball after drying；
Described in step (1), the preparation method of double-deck modification nano ferriferrous oxide magnetic fluid is:
A, it is 1.9:1 ~ 2.1:1 in molar ratio, weighs iron chloride and ferrous chloride, feed the mixture in the ratio of 5 ~ 50g/L and obtain mixed liquor in the distilled water of nitrogen deoxidation；
B, weigh internal layer dressing agent stearic acid and add in mixed liquor, wherein the mol ratio 1:2 ~ 1:6 of stearic acid and iron ion；Regulate bath temperature be 60 ~ 90 DEG C, then in mixed liquor add ammonia, the PH making solution is 8 ~ 10, react 20 ~ 40min, obtain monolayer modify nano ferriferrous oxide, wash three times stand-by；
In C, the ultrasonic beaker being dissolved in distilled water of outer layer dressing agent weighed in the ratio of 0.5g/L, mol ratio 1:1 ~ the 6:1 of its ectomesoderm dressing agent and iron ion, it is that the ratio of 1:4 ~ 1:6 is by above-mentioned monolayer modification nano ferriferrous oxide addition outer layer dressing agent solution by volume, supersound process 10 minutes, obtains double-deck modification nano ferriferrous oxide magnetic fluid；
Described outer layer dressing agent is the one in sorbitol, cetyl trimethylammonium bromide, Polyethylene Glycol。
2. the preparation method of magnetic hydroxylapatite crystal whisker ball according to claim 1, it is characterised in that: the acidity-basicity regulator in course of reaction is carbamide, and it is concentrated nitric acid that the pH value of initial condition regulates the acid solution used。
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| CN102614549A (en) * | 2012-03-07 | 2012-08-01 | 北京化工大学 | Ferroferric oxide calcium phosphate nuclear shell magnetic nanoparticle and preparation method thereof by biological mineralization method |
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