CN109133022A - A kind of hydroxyapatite nano-structure of morphology controllable, preparation method and application - Google Patents
A kind of hydroxyapatite nano-structure of morphology controllable, preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of hydroxyapatite nano-structure of morphology controllable, preparation method and applications, belong to Inorganic synthese field of material technology.It is prepared the following steps are included: raw material phosphorus pentoxide dispersant liquid drop is added to solubility calcium saline solution, and dispersion liquid used is the organic solvents such as alcohol, ether, ketone, DMF；Phosphorus pentoxide and soluble calcium salt form hydroxyapatite presoma in the solution；Regulate and control hydroxyapatite presoma nanostructure using the pH value of reaction medium；Hydro-thermal process is carried out to presoma.Using the above scheme, the present invention can obtain the hydroxyapatite nano-structure of morphology controllable, products obtained therefrom can be applicable to the fields such as soil remediation, water process, biological medicine.
Description
Technical field
The invention belongs to Inorganic synthese field of material technology more particularly to a kind of hydroxyapatite nano knots of morphology controllable
Structure, preparation method and application.
Background technique
Hydroxyapatite (Hydroxyapatite, HAP) belongs to one kind of apatite mineral, special crystal structure
Feature makes it have good ion-exchange performance, has to most of heavy metal ion, fluorine ion and organic pollutant good
Good absorption fixed function, and it is good with the harmony of environment, secondary pollution is not easily caused, to become a kind of novel environmental function
Material is for the reparation of contaminated soil and the improvement of water body.
Hydroxyapatite also has good bioactivity and biocompatibility, is a kind of excellent bioactive materials,
Biologically active artificial bone, high-quality toothpaste abrasives, in terms of application it is more.
As people go deep into hydroxyapatite research, nanometer hydroxyapatite is in catalytic carrier, ion exchange, biology
Medicine and other fields are widely used, so as to cause the great interest of people and concern.Then, various pattern hydroxyls are synthesized
The method of apatite nano material is come into being, and two class of dry and wet is broadly divided into.Wherein wet process is divided into the precipitation method, hydro-thermal again
Method, microemulsion method and sol-gel method.
The present invention is prepared for the hydroxyapatite nano-structure of different-shape using hydro-thermal method, and preparation method is easy, repeats
Property is strong.
Summary of the invention
The purpose of the present invention is to provide a kind of hydroxyapatite nano-structure of morphology controllable, preparation method and answer
With the present invention synthesizes the hydroxyapatite nano-structure of different-shape by Control experiment condition.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, which is characterized in that steps are as follows:
(1) by P2O5It is scattered in organic media and obtains P2O5Dispersion liquid, P2O5Mass fraction in organic media is 0.2%-
3%；
(2) soluble calcium salt is dispersed in water, the mass fraction of calcium salt in water is 1%-20%；
(3) by P2O5Dispersion liquid adds in calcium saline solution, and tune pH is 4-10.0, continues 20 ~ 40 min of stirring, then continues at height
It presses in reaction kettle, in 110-200 DEG C of reaction 6-24 h, precipitates after ethyl alcohol, water washing, 50-80 DEG C of drying is received to get to HAP
Mitron or nanosphere.Obtained hydroxyapatite nano Guan Kuanwei 12-40 nm, long 22-395 nm；Nanosphere is (spongy, more
Hole) partial size be 23-130 nm.
Further, for ethyl alcohol, methanol, ether, acetone or DMF(, its effect is control phosphorus pentoxide to organic media
Hydrolysis), soluble calcium salt is calcium chloride or calcium nitrate.
Further, step (3) is by P2O5Feed way when dispersion liquid is added in calcium saline solution is by P2O5Dispersion liquid
It is transferred to constant pressure funnel, is then added dropwise in calcium saline solution with 5-30 drop/min rate of addition.
Further, the ammonium hydroxide or organic amine (specific such as triethylamine, ethylenediamine) when pH are adjusted.
Hydroxyapatite nano-structure made from above-mentioned preparation method.
Application of the above-mentioned hydroxyapatite nano-structure in absorption heavy metal ion, the hydroxyapatite nano-structure
For wide 12-31 nm, the nanotube of long 22-368 nm, the heavy metal ion is Pb2+、Cd2+、AsO4 3-。
Application of the above-mentioned hydroxyapatite nano-structure in absorption heavy metal ion, the hydroxyapatite nano-structure
For partial size 33-80 nm nanosphere, the heavy metal ion is Pb2+、Cd2+、Co2+、Hg2+、Cu2+、Zn2+、Ni2+。
Using the above scheme, the hydroxyapatite nano-structure of available morphology controllable, products obtained therefrom can be applicable to soil
The fields such as earth reparation, water process, biological medicine.Product made from the above method is porous, large specific surface area, non-stimulated and safe.
Detailed description of the invention
It in pH is 4.0(Fig. 1 a that Fig. 1, which is embodiment 1), 7.5(Fig. 1 b), 8.3(Fig. 1 c), 8.8(Fig. 1 d), 9.5(Fig. 1 e)
The TEM of obtained HAP schemes, and the scale size of each figure is 50nm in Fig. 1；
Fig. 2 is embodiment 2 in 3 DEG C (Fig. 2 a), 10 DEG C (Fig. 2 b), 17 DEG C (Fig. 2 c), 24 DEG C (Fig. 2 d), 31 DEG C (Fig. 2 e) stirring temperature
The lower TEM for preparing HAP of degree schemes, and b icon ruler size is 20nm in Fig. 2, other figures are then 50nm；
Fig. 3 is the TEM figure for the HAP nanotube that embodiment 3 obtains；
Fig. 4 is the TEM figure for the HAP nanotube that embodiment 4 obtains；
Fig. 5 is the TEM figure for the HAP nanotube that embodiment 5 obtains；
Fig. 6 is the TEM figure for the spongy HAP nanosphere different amplification that embodiment 6 obtains, and a icon ruler size is 50nm,
B icon ruler size is 20nm；
Fig. 7 is the N for the spongy HAP nanosphere that embodiment 6 obtains2Adsorption-desorption curve；
Fig. 8 is the TEM figure for the HAP nanoporous ball that embodiment 7 obtains；
Fig. 9 is the SEM figure for the HAP nanometer stub that embodiment 8 obtains；
Figure 10 is the XRD diagram for the HAP nanoporous ball that embodiment 7 obtains；
Figure 11 is the obtained HAP nanotube of embodiment 4 in the solution to Pb2+、Cd2+、AsO4 3-Adsorption rate comparison diagram；
Figure 12 be the obtained spongy HAP of embodiment 7 in mixed solution to Pb2+、Cd2+、Co2+、Hg2+、Cu2+、Zn2+、Ni2+
Adsorption rate comparison diagram.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below, but protection model of the invention
It encloses and is not limited thereto.
Embodiment 1
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
By 0.20 g P2O5It is added to 2 min of ultrasonic disperse in 15 mL dehydrated alcohols, while taking 1.20 g Ca (NO3)2It is added
It is dissolved into 15 mL water, at room temperature by P2O5Ca (NO is slowly dropped into alcohol mixeding liquid3)2In aqueous solution (13 drops/
), and magnetic agitation min.Prepare 6 parts of solution simultaneously according to the method described above.6 parts of solution are then used into concentrated ammonia liquor (25 ~ 28wt%) point
Not Tiao pH be 4.0,7.5,8.3,8.8,9.5,10.0, continue in 17 DEG C of 30 min of stirring, be transferred to autoclave, 165 DEG C after
12 h of continuous reaction.Naturally after being cooled to room temperature, precipitating dehydrated alcohol, water are respectively washed 3 times, obtain HAP solid in 60 DEG C of drying.In pH
The HAP pattern obtained for 4.0,7.5,8.3,8.8,9.5 is respectively loose spherical shape (Fig. 1 a), porous ball (Fig. 1 b), medicine ball
(Fig. 1 c), nanotube (Fig. 1 d), spongy (Fig. 1 e).
Embodiment 2
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
By 0.20 g P2O5It is added 2 min of ultrasonic disperse in 15 mL dehydrated alcohols, and by 1.20 g Ca (NO3)2It is dissolved in 15 mL
In water, by P at 17 DEG C2O5Ca (NO is slowly dropped into alcohol mixeding liquid3)2In aqueous solution (12 drops/min), and magnetic agitation.
It is then 8.8 with concentrated ammonia liquor tune pH, 5 parts of samples is prepared simultaneously according to the method described above, respectively in 3 DEG C, 10 DEG C, 17 DEG C, 24 DEG C, 31
DEG C 30 min of stirring, are transferred to autoclave, 165 DEG C of the reaction was continued 12 h.Naturally after being cooled to room temperature, precipitating dehydrated alcohol,
Water is respectively washed 3 times, obtains HAP solid in 60 DEG C of drying.It is equal in the HAP pattern that 3 DEG C, 10 DEG C, 17 DEG C, 24 DEG C, 31 DEG C stir to get
To be nanotube-shaped, pipe range, pipe it is wide be respectively 30-190 nm, 17-37 nm(Fig. 2 a), 44-130 nm, 17-31 nm(Fig. 2 b),
43-186 nm, 12-30 nm(Fig. 2 c), 63-250 nm, 15-33 nm(Fig. 2 d) and 24-352 nm, 13-30 nm(Fig. 2 e).
Embodiment 3
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
By 0.20 g P2O5It is added to 2 min of ultrasonic disperse in 15 mL ether, by 1.20 g Ca (NO3)2It is dissolved in 15 mL water
In, by P at 10 DEG C2O5Ca (NO is slowly dropped into ether mixed liquor3)2In aqueous solution (5 drops/min), and magnetic agitation.Then use
Concentrated ammonia liquor tune pH is 8.8, is continued in 10 DEG C of 30 min of stirring, is transferred to autoclave, 165 DEG C of the reaction was continued 12 h.Naturally cold
To room temperature, precipitating dehydrated alcohol, water are respectively washed 3 times, obtain HAP solid in 60 DEG C of drying.As shown in figure 3, obtained HAP is
Nanotube-shaped, width is 13-29 nm, a length of 55-395 nm.
Embodiment 4
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
By 0.03 g P2O5It is added to ultrasonic disperse in 15 mL methanol, takes 0.15 g CaCl2Water is added to molten in 15 mL water
Solution, by P in 31 DEG C of water-baths2O5/ methyl alcohol mixed liquor is slowly dropped into CaCl2In aqueous solution (11 drops/min), and magnetic agitation.With
It is afterwards 8.8 with triethanolamine tune pH, continues to be transferred to autoclave, 110 DEG C the reaction was continued in 31 DEG C of 30 min of stirred in water bath
24 h.Naturally after being cooled to room temperature, precipitating dehydrated alcohol, water are respectively washed 3 times, obtain HAP solid in 50 DEG C of drying.As shown in figure 4,
Obtained HAP be it is nanotube-shaped, width be 12-31 nm, a length of 22-368 nm.
Three parts of HAP nanotube are weighed in 0.1 g embodiment 4 in parallel, is separately added into 30 mL Pb2+(initial concentration 160
mg·L-1), 30 mL Cd2+(initial concentration is 170 mgL-1), 30 mL AsO4 3-(initial concentration is 60 mgL-1) solution
In, it after evenly dispersed, is centrifuged after 2 h of shaken at room temperature, takes supernatant and carry out ICP detection.As a result as shown in figure 11, HAP nanometers
Pipe is to Pb2+、Cd2+、AsO4 3-The adsorption rate of ion is respectively 100%, 98.7%, 81.4%, to three heavy metal species ions in solution
All have preferable adsorption capacity.
Embodiment 5
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
By 0.20 g P2O5It is added in 15 mL acetone, takes 1.20 g CaCl2It is added in 15 mL water and dissolves, 3 DEG C will
P2O5/ acetone mixture is slowly dropped into CaCl2In aqueous solution (7 drops/min), and magnetic agitation.Then it is with concentrated ammonia liquor tune pH
8.8, continue in 3 DEG C of 30 min of stirring, is transferred to autoclave, 165 DEG C of the reaction was continued 12 h.Naturally after being cooled to room temperature, precipitating
It is respectively washed 3 times with dehydrated alcohol, water, obtains HAP solid in 60 DEG C of drying.As shown in figure 5, obtained HAP be it is nanotube-shaped, width is
14-38 nm, a length of 52-186 nm.
Embodiment 6
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
0.45 g P2O5It is added in 15 mL acetone, takes 3.00 g CaCl2It is added in 15 mL water and dissolves, it will at 17 DEG C
P2O5/ acetone mixture is slowly dropped into CaCl2In aqueous solution (30 drops/min), and magnetic agitation.Then it is with ethylenediamine tune pH
9.5, continue in 17 DEG C of 30 min of stirring, is transferred to autoclave, 200 DEG C of the reaction was continued 6 h.Naturally after being cooled to room temperature, precipitating
It is respectively washed 3 times with dehydrated alcohol, water, obtains HAP solid in 80 DEG C of drying.As shown in fig. 6, obtained HAP be it is fluffy spongy,
Partial size is 23-72 nm, as shown in fig. 7, specific surface area is 70.92 m2/g。
Embodiment 7
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
0.204 g P2O5It is added in 15 mL ether, takes 0.24 g Ca (NO3)2It is added in 15 mL water and dissolves, at 18 DEG C
By P2O5/ ether mixed liquor is slowly dropped into Ca (NO3)2In aqueous solution (10 drops/min), and magnetic agitation.Then with concentrated ammonia liquor tune
PH is 10.0, is continued in 18 DEG C of 30 min of stirring, is transferred to autoclave, 165 DEG C of the reaction was continued 12 h.Naturally it is cooled to room temperature
Afterwards, precipitating dehydrated alcohol, water are respectively washed 3 times, obtain HAP solid in 60 DEG C of drying.Obtained HAP is porous ball, such as Fig. 8 institute
Show, porous ball partial size is 33-80 nm.Figure 10 is the XRD spectra of porous spherical HAP, it can be seen from the figure that the HAP of preparation exists
2 theta are the characteristic diffraction peak of hydroxyapatite occur at 25.8,31.7,32.2,39.7,46.7,49.3, are respectively corresponded
(002), (211), (112), (310), (222) and (213) 6 crystal faces, with standard JCPDS card (PDF 46-0905) one
It causes, illustrates that the product of preparation is HAP.
Weighing HAP made from 0.50 g embodiment 7 is porous ball, and 30 mL are added and contain Pb2+、Cd2+、Co2+、Hg2+、Cu2+、
Zn2+、Ni2+Mixed solution (initial concentration of every metal ion species is 20 mgL-1) solution, after 2 h of shaken at room temperature from
The heart takes supernatant to survey ICP.As a result as shown in figure 12, HAP porous ball is to Pb2+、Cd2+、Co2+、Hg2+、Cu2+、Zn2+、Ni2+Ion
Adsorption rate is respectively 99.6%, 30.6%, 100%, 95.0%, 99.4%, 100%, 99.9%, to the heavy metal ion in mixed solution
All have preferable adsorption capacity.
Embodiment 8
A kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, steps are as follows:
0.40 g P2O5It is added in 15 mLDMF, takes 2.40 g Ca (NO3)2It is added in 15 mL water and dissolves, it will at 27 DEG C
P2O5/ DMF mixed liquor instills Ca (NO3)2In aqueous solution (8 drops/min), and magnetic agitation.It is then 10.0 with concentrated ammonia liquor tune pH,
Continue in 27 DEG C of 30 min of stirring, is transferred to autoclave, 165 DEG C of the reaction was continued 12 h.Naturally after being cooled to room temperature, precipitating uses nothing
Water-ethanol, water are respectively washed 3 times, are dried in 70 DEG C of baking ovens, are obtained HAP solid.Obtained HAP is corynebacterium, as shown in figure 9, stick
A length of 48-152 nm, width are 38-105 nm.
Claims (9)
1. a kind of preparation method of the hydroxyapatite nano-structure of morphology controllable, which is characterized in that steps are as follows:
(1) by P2O5It is scattered in organic media and obtains P2O5Dispersion liquid, P2O5Mass fraction in organic media is 0.2%-
3%；
(2) soluble calcium salt is dispersed in water, the mass fraction of calcium salt in water is 1%-20%；
(3 by P2O5Dispersion liquid adds in calcium saline solution, and tune pH is 4-10.0, continues 20 ~ 40 min of stirring, then continues at high pressure
In reaction kettle, in 110-200 DEG C of reaction 6-24 h, precipitate it is washed, dry after to get arriving HAP nanotube or nanosphere.
2. the preparation method of the hydroxyapatite nano-structure of morphology controllable according to claim 1, it is characterised in that:
Hydroxyapatite nano Guan Kuanwei the 12-40 nm, long 22-395 nm arrived；Nanosphere partial size is 23-130 nm.
3. the preparation method of the hydroxyapatite nano-structure of morphology controllable according to claim 1, it is characterised in that: have
Machine medium is ethyl alcohol, methanol, ether, acetone or DMF, and soluble calcium salt is calcium chloride or calcium nitrate.
4. the preparation method of the hydroxyapatite nano-structure of morphology controllable according to claim 1, it is characterised in that: step
Suddenly (3) are by P2O5Feed way when dispersion liquid is added in calcium saline solution is by P2O5Dispersion liquid is with 5-30 drop/min dropwise addition
Speed is added dropwise in calcium saline solution.
5. the preparation method of the hydroxyapatite nano-structure of morphology controllable according to claim 1, it is characterised in that: adjust
Ammonium hydroxide or organic amine when pH.
6. the preparation method of the hydroxyapatite nano-structure of morphology controllable according to claim 1, which is characterized in that institute
Stating the drying temperature in step (3) is 50-80 DEG C.
7. hydroxyapatite nano-structure made from any preparation method of claim 1 to 6.
8. application of the hydroxyapatite nano-structure described in claim 7 in absorption heavy metal ion, which is characterized in that described
Hydroxyapatite nano-structure is width 12-31 nm, and the nanotube of long 22-368 nm, the heavy metal ion is Pb2+、Cd2+、
AsO4 3-。
9. application of the hydroxyapatite nano-structure described in claim 7 in absorption heavy metal ion, which is characterized in that described
Hydroxyapatite nano-structure is partial size 33-80 nm nanosphere, and the heavy metal ion is Pb2+、Cd2+、Co2+、Hg2+、Cu2+、
Zn2+、Ni2+。
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Cited By (3)
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| CN111978097A (en) * | 2020-08-28 | 2020-11-24 | 四川大学 | Bone-induced calcium phosphate ceramic with hollow tube structure and preparation method thereof |
| CN114797915A (en) * | 2022-04-15 | 2022-07-29 | 苏州大学 | Hydroxyapatite, preparation method thereof and application of hydroxyapatite in piezoelectric catalytic degradation of organic pollutants in water |
| CN117229561A (en) * | 2023-11-10 | 2023-12-15 | 中裕软管科技股份有限公司 | Polyurethane toughening modified multifunctional composite material with porous structure and preparation method thereof |
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| CN111978097A (en) * | 2020-08-28 | 2020-11-24 | 四川大学 | Bone-induced calcium phosphate ceramic with hollow tube structure and preparation method thereof |
| CN114797915A (en) * | 2022-04-15 | 2022-07-29 | 苏州大学 | Hydroxyapatite, preparation method thereof and application of hydroxyapatite in piezoelectric catalytic degradation of organic pollutants in water |
| WO2023197385A1 (en) * | 2022-04-15 | 2023-10-19 | 苏州大学 | Hydroxyapatite and preparation method therefor, and application thereof in piezoelectric catalytic degradation of organic pollutant in water |
| CN117229561A (en) * | 2023-11-10 | 2023-12-15 | 中裕软管科技股份有限公司 | Polyurethane toughening modified multifunctional composite material with porous structure and preparation method thereof |
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