CN108584898A - A method of preparing small size nanometer hydroxyapatite by template of carbon dots - Google Patents
A method of preparing small size nanometer hydroxyapatite by template of carbon dots Download PDFInfo
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- CN108584898A CN108584898A CN201810728809.4A CN201810728809A CN108584898A CN 108584898 A CN108584898 A CN 108584898A CN 201810728809 A CN201810728809 A CN 201810728809A CN 108584898 A CN108584898 A CN 108584898A
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/325—Preparation by double decomposition
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- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The invention belongs to nano meter biomaterial fields, disclose a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots.Weigh H2N(CH2)10COOH and NaOH solids are dissolved in deionized water, are added citric acid solution and are stirred to react, and collect white precipitate drying, grinding, then the thermal oxidative reaction at a temperature of 300 DEG C, obtains CDs；Ca (NO are adjusted with aqueous slkali3)2Then pH value of solution is added dropwise CDs and carries out complex-precipitation reaction, then Na is added dropwise to 10.53PO4Solution, hydro-thermal reaction at a temperature of 140~180 DEG C, product is washed, dry, obtains small size nanometer hydroxyapatite.Hydroxyapatite nanoparticle prepared by the present invention is in corynebacterium, and size ratio is small without particle size existing for carbon dots, and the increase of carbon dots content can effectively reduce the size of particle, has potential application prospect in nanometer field of medicaments.
Description
Technical field
The invention belongs to nano meter biomaterial fields, and in particular to a kind of to prepare small size nano-hydroxy by template of carbon dots
The method of apatite.
Background technology
Hydroxyapatite is a kind of bioactive materials, has mineralogical composition similar with skeleton, is possessed good
Biocompatibility.In addition, hydroxyapatite also has preferable osteoconductive, it is made to be answered extensively in biomedical sector
For human body hard tissue damage and the reparation of defect, replacement etc..
In recent years, hydroapatite particles are also widely applied in terms of the transmission of drug, albumen, nucleic acid etc..So
And some are the study found that nano-grade hydroxy apatite has many advantages, such as that size is small, large specific surface area, itself can be used as inhibition
Cancer cell multiplication, the Nano medication for promoting cancer cell-apoptosis.The various sizes of nano hydroxyapatite of existing literature and document announcement
The anticarcinogenic effect of lime stone difference, but control group is only conceived to the difference of size, fails to keep this variable of grain shape
Consistency.
The hydroapatite particles prepared at present by template are generally spherical in shape, and size is mostly in 200nm or more, no
It is suitable for analyzing very much influence of the dimensional effect to cancer cell of nano particle.
Invention content
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing one kind with carbon
Point is the method that template prepares small size nanometer hydroxyapatite.The carbon dots (CDs) of functionalization are the class ball that grain size is less than 10nm
Shape particle, and a large amount of-COO is contained on surface-Group, can effectively and Ca2+Coordination bonding can be used as synthesis small size hydroxyl phosphorus
The ideal template of lime stone nano particle.
Another object of the present invention is to provide a kind of nanometer hydroxyapatites being prepared by the above method.The party
Nanometer hydroxyapatite prepared by method is in corynebacterium, and particle diameter distribution is more uniform.
The object of the invention is achieved through the following technical solutions：
A method of preparing small size nanometer hydroxyapatite, including following preparation process by template of carbon dots：
(1) preparation of carbon dots (CDs)：
Weigh H2N(CH2)10COOH and NaOH solids, are dissolved in deionized water, and centrifugation removal impurity then adds lemon
Lemon acid solution, is stirred to react, and collects white precipitate drying, grinding, then the thermal oxidative reaction at a temperature of 300 DEG C, obtains carbon dots
Product (CDs)；
(2) preparation of small size nanometer hydroxyapatite：
Ca (NO are adjusted with aqueous slkali3)2PH value of solution to 10.5, the then CDs of a dropping step (1) carry out complex-precipitation reaction,
Na is added dropwise again3PO4Solution, hydro-thermal reaction at a temperature of 140~180 DEG C, product is washed, dry, obtains small size nano hydroxyapatite
Lime stone.
Preferably, H described in step (1)2N(CH2)10The molar ratio of COOH and NaOH solids is 1:1.
Preferably, the addition and H of citric acid described in step (1)2N(CH2)10The molar ratio of COOH is 1:1.
Preferably, the time being stirred to react described in step (1) is 30~45min.
Preferably, carbon dots product described in step (1) further purifies by the following method：By gained carbon dots product ultrasound
In deionized water, centrifugation removal infusible precipitate is then molten with the bag filter dialysis product that molecular cut off is 3500D for dissolving
24~48h of liquid is freeze-dried the carbon dots product purified.
Preferably, aqueous slkali described in step (2) refers to the NaOH solution of 0.5~1mol/L.
Preferably, the addition of CDs described in step (2) makes it (Na be added dropwise in calcium phosphorus reaction solution3PO4Reaction afterwards is molten
Liquid) in content be 0.22~1.11g/L.
Preferably, Ca (NO in step (2)3)2With Na3PO4The molar ratio of addition is 5:3.
Preferably, the time of hydro-thermal reaction described in step (2) is 6~10h.
Preferably, washing described in step (2) refers to being washed with deionized water and ethyl alcohol, and the drying refers to 50~60
DEG C drying.
A kind of nanometer hydroxyapatite, is prepared by the above method.
The present invention preparation method and obtained product has the following advantages that and advantageous effect：
Hydroxyapatite nanoparticle prepared by the present invention is in corynebacterium, and size ratio is small without particle size existing for carbon dots,
And the increase of carbon dots content can effectively reduce the size of particle, have potential application prospect in nanometer field of medicaments.
Description of the drawings
Fig. 1 is the transmission of the nanometer hydroxyapatite of different carbon dots contents prepared by comparative example of the present invention and Examples 1 to 3
Electron microscope (TEM).
Fig. 2 is the X ray diffracting spectrum (XRD) of nanometer hydroxyapatite prepared by comparative example of the present invention and Examples 1 to 3
With hydroxyapatite standard diagram (JCPDS 09-0432) compares figure.
Fig. 3 is the Fourier transform infrared spectroscopy of nanometer hydroxyapatite prepared by comparative example of the present invention and Examples 1 to 3
Scheme (FTIR).
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Comparative example
The preparation for the nanometer hydroxyapatite that this comparative example is added without template：
Ca (the NO of a concentration of 0.5mol/L of 10mL are measured first3)2Solution, deionized water are diluted to 25mL, are then used
The NaOH solution of 1mol/L adjusts Ca (NO3)2The pH to 10.5 of solution；Then a concentration of 0.1mol/ of 30mL are slowly added dropwise thereto
The Na of L3PO4Solution；Then mixed liquor is transferred in polytetrafluoroethylene (PTFE) autoclave, 8h is reacted under 180 DEG C of hydrothermal conditions, it is natural
It is cooled to room temperature, deionized water and ethyl alcohol clean 3 times, and dry in 50 DEG C of baking ovens, grind to obtain nanometer hydroxyapatite S1.
Embodiment 1
(1) preparation of carbon dots (CDs)：
In molar ratio 1:1 weighs H2N(CH2)10COOH and NaOH solids are added 25mL deionized waters and neutralize, centrifugation removal
Impurity.Then add 25mL and H2N(CH2)10The citric acid solution of COOH equimolar concentrations is vigorously stirred 30min, collects white
Color precipitates drying；Finally drying sample is ground, is positioned over 300 DEG C of Muffle furnaces, thermal oxidative reaction 2h, natural cooling is taken out；Heat
Product utilization ultrasonic method after oxidation is dissolved in deionized water, centrifugation removal infusible precipitate, after use molecular cut off
For the bag filter dialysis reaction mixture 48h of 3500D, the carbon dots product for being freeze-dried to purify.
(2) preparation of small size nanometer hydroxyapatite：
Ca (the NO of a concentration of 0.5mol/L of 10mL are measured first3)2Solution, deionized water are diluted to 24.5mL, then use
The NaOH solution of 1mol/L adjusts Ca (NO3)2PH value of solution is to 10.5.A concentration of 24.4g/L of 0.5mL are then slowly added dropwise thereto
CDs, holding calcium source liquor capacity be 25mL, a concentration of 0.2mol/L；It waits for that CDs-Ca complex-precipitations are uniformly dispersed, is slowly added dropwise
The Na of a concentration of 0.1mol/L of 30mL3PO4Solution；Then mixed liquor is transferred in polytetrafluoroethylene (PTFE) autoclave, in 180 DEG C of hydro-thermals
Under the conditions of react 8h, cooled to room temperature, deionized water and ethyl alcohol clean 3 times, and dry in 50 DEG C of baking ovens, grind small
Sized nanostructures hydroxyapatite S2.
Embodiment 2
(1) preparation of carbon dots (CDs) is the same as embodiment 1.
(2) preparation of small size nanometer hydroxyapatite：
Ca (the NO of a concentration of 0.5mol/L of 10mL are measured first3)2Solution, deionized water are diluted to 23.5mL, then use
The NaOH solution of 1mol/L adjusts Ca (NO3)2PH value of solution is to 10.5.A concentration of 24.4g/L of 1.5mL are then slowly added dropwise thereto
CDs, holding calcium source liquor capacity be 25mL, a concentration of 0.2mol/L；It waits for that CDs-Ca complex-precipitations are uniformly dispersed, is slowly added dropwise
The Na of a concentration of 0.1mol/L of 30mL3PO4Solution；Then mixed liquor is transferred in polytetrafluoroethylene (PTFE) autoclave, in 180 DEG C of hydro-thermals
Under the conditions of react 8h, cooled to room temperature, deionized water and ethyl alcohol clean 3 times, and dry in 50 DEG C of baking ovens, grind small
Sized nanostructures hydroxyapatite S3.
Embodiment 3
(1) preparation of carbon dots (CDs) is the same as embodiment 1.
(2) preparation of small size nanometer hydroxyapatite：
Ca (the NO of a concentration of 0.5mol/L of 10mL are measured first3)2Solution, deionized water are diluted to 22.5mL, then use
The NaOH solution of 1mol/L adjusts Ca (NO3)2PH value of solution is to 10.5.A concentration of 24.4g/L of 2.5mL are then slowly added dropwise thereto
CDs, holding calcium source liquor capacity be 25mL, a concentration of 0.2mol/L；It waits for that CDs-Ca complex-precipitations are uniformly dispersed, is slowly added dropwise
The Na of a concentration of 0.1mol/L of 30mL3PO4Solution；Then mixed liquor is transferred in polytetrafluoroethylene (PTFE) autoclave, in 180 DEG C of hydro-thermals
Under the conditions of react 8h, cooled to room temperature, deionized water and ethyl alcohol clean 3 times, and dry in 50 DEG C of baking ovens, grind small
Sized nanostructures hydroxyapatite S4.
The transmission electron microscope picture of the nanometer hydroxyapatite of different carbon dots contents prepared by the above comparative example and Examples 1 to 3
(TEM) as shown in Figure 1.As can be seen from the figure under the conditions of existing for no carbon dots, the size ratio of particle contains the particle of carbon dots
Size is slightly larger, and is all in rodlike, complete crystallization.
The X ray diffracting spectrum (XRD) and hydroxyl of nanometer hydroxyapatite prepared by the above comparative example and Examples 1 to 3
Apatite standard diagram (JCPDS 09-0432) compares figure is as shown in Figure 2.Embodiment sample is the hydroxyl of pure phase as can be seen from Figure
Base apatite, when carbon dots content increases in sample, gradually widthization, intensity slightly reduce diffraction maximum.As a whole, embodiment sample
The crystallization of product is all more perfect.
The Fourier transform infrared spectroscopy figure of nanometer hydroxyapatite prepared by the above comparative example and Examples 1 to 3
(FTIR) as shown in Figure 3.With the increase of carbon dots content, CO3 2-Absorption peak strength gradually increase, for Type B substitution carbonic acid phosphorus
Lime stone.As a result it can be explained, carbon dots can be used as template, and CO can be also introduced into hydroapatite particles3 2-Group, substitution portion
Divide PO4 3-, to subtract short grained size.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots, it is characterised in that including preparing step as follows
Suddenly：
(1) preparation of CDs：
Weigh H2N(CH2)10COOH and NaOH solids, are dissolved in deionized water, and it is molten then to add citric acid for centrifugation removal impurity
Liquid is stirred to react, and collects white precipitate drying, grinding, then the thermal oxidative reaction at a temperature of 300 DEG C, obtains CDs；
(2) preparation of small size nanometer hydroxyapatite：
Ca (NO are adjusted with aqueous slkali3)2For pH value of solution to 10.5, then the CDs of a dropping step (1) carries out complex-precipitation reaction, then drips
Add Na3PO4Solution, hydro-thermal reaction at a temperature of 140~180 DEG C, product is washed, dry, obtains small size nano-hydroxy-apatite
Stone.
2. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：H described in step (1)2N(CH2)10The molar ratio of COOH and NaOH solids is 1:1.
3. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：The addition and H of citric acid described in step (1)2N(CH2)10The molar ratio of COOH is 1:1.
4. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：The time being stirred to react described in step (1) is 30~45min.
5. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is that carbon dots product described in step (1) further purifies by the following method：Gained carbon dots product ultrasonic dissolution is being gone
In ionized water, centrifugation removal infusible precipitate, then with molecular cut off be 3500D bag filter dialysis reaction mixture 24~
48h is freeze-dried the carbon dots product purified.
6. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：Aqueous slkali described in step (2) refers to the NaOH solution of 0.5~1mol/L.
7. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：The addition of CDs described in step (2) makes its content in calcium phosphorus reaction solution be 0.22~1.11g/L.
8. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：Ca (NO in step (2)3)2With Na3PO4The molar ratio of addition is 5:3.
9. a kind of method preparing small size nanometer hydroxyapatite as template using carbon dots according to claim 1, special
Sign is：The time of hydro-thermal reaction described in step (2) is 6~10h；The washing refers to being washed with deionized water and ethyl alcohol,
The drying refers to being dried at 50~60 DEG C.
10. a kind of nanometer hydroxyapatite, it is characterised in that：It is prepared by claim 1~9 any one of them method
It arrives.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078037A (en) * | 2019-05-23 | 2019-08-02 | 哈尔滨理工大学 | A kind of synthetic method with spherical morphology hydroxyapatite nanoparticle |
| CN112093788A (en) * | 2020-09-06 | 2020-12-18 | 桂林理工大学 | Preparation method and application of cadmium-calcium-fluorapatite solid solution |
| CN113307240A (en) * | 2021-05-28 | 2021-08-27 | 华南理工大学 | Nano-hydroxyapatite particles with anti-tumor activity and preparation method thereof |
| CN114275751A (en) * | 2022-02-16 | 2022-04-05 | 湖南大学 | Preparation method of hexagonal macroporous hydroxyapatite, product and application thereof |
| CN114751397A (en) * | 2022-03-29 | 2022-07-15 | 华南师大(清远)科技创新研究院有限公司 | Fluorescent nano hydroxyapatite and preparation method and application thereof |
| CN116656350A (en) * | 2023-03-28 | 2023-08-29 | 华南理工大学 | Solid single-particle dispersed carbon dots, and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110078037A (en) * | 2019-05-23 | 2019-08-02 | 哈尔滨理工大学 | A kind of synthetic method with spherical morphology hydroxyapatite nanoparticle |
| CN110078037B (en) * | 2019-05-23 | 2022-08-16 | 哈尔滨理工大学 | Synthetic method of hydroxyapatite nanoparticles with spherical morphology |
| CN112093788A (en) * | 2020-09-06 | 2020-12-18 | 桂林理工大学 | Preparation method and application of cadmium-calcium-fluorapatite solid solution |
| CN113307240A (en) * | 2021-05-28 | 2021-08-27 | 华南理工大学 | Nano-hydroxyapatite particles with anti-tumor activity and preparation method thereof |
| CN114275751A (en) * | 2022-02-16 | 2022-04-05 | 湖南大学 | Preparation method of hexagonal macroporous hydroxyapatite, product and application thereof |
| CN114751397A (en) * | 2022-03-29 | 2022-07-15 | 华南师大(清远)科技创新研究院有限公司 | Fluorescent nano hydroxyapatite and preparation method and application thereof |
| CN114751397B (en) * | 2022-03-29 | 2024-06-21 | 华南师大(清远)科技创新研究院有限公司 | Fluorescent nano hydroxyapatite and preparation method and application thereof |
| CN116656350A (en) * | 2023-03-28 | 2023-08-29 | 华南理工大学 | Solid single-particle dispersed carbon dots, and preparation method and application thereof |
| CN116656350B (en) * | 2023-03-28 | 2024-04-26 | 华南理工大学 | Solid single-particle dispersed carbon dots, and preparation method and application thereof |
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Application publication date: 20180928 |