CN109502565A - The method that one-step method prepares Oil soluble hydroxy apatite nanometer rods - Google Patents
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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Abstract
The present invention relates to a kind of preparation method of one-step method Oil soluble hydroxy apatite nanometer rods, solution A is obtained by soluble calcium salt is soluble in water；Water soluble alkali, which is dissolved in the mixed liquor of ethyl alcohol and oleic acid, obtains solution B；Solution B is added dropwise in three-necked flask, solution A is slowly added dropwise under stirring condition and obtains solution C；Soluble phosphate is soluble in water to obtain solution D；Solution D is added drop-wise in solution C, stirs to get suspension；Water soluble alkali solution instills in suspension and obtains mixed liquor；Mixed liquor reacts at 80-180 DEG C in high-temperature high-pressure reaction kettle, is cooled to room temperature and obtains reaction solution；Reaction solution is centrifugally separating to obtain sediment, is washed using dehydrated alcohol and hexamethylene alternating centrifugal, obtains Oil soluble hydroxy apatite nanometer rods.Raw material sources of the present invention are rich and easy to get, low in cost, and synthesis technology is simple, good process repeatability；Product quality is stable and morphology controllable is good, good dispersion；The fields such as bio-medical material and coating material can be widely used in.
Description
Technical field
The invention belongs to inorganic nano material technology of preparing, especially a kind of one-step method prepares Oil soluble hydroxy apatite and receives
The method of rice stick
Background technique
Hydroxyapatite, abbreviation HA, chemical molecular formula Ca10(PO4)6(OH)2, nanocrystal is in hexagonal crystal system, structure
For hexagonal prism body.Hydroxyapatite and natural bone have similar chemical component, have excellent biological nature, and crystal has very by force
Ionic compartmentation, be therefore widely used in bone substitution or reparation, pharmaceutical carrier, fluorescent marker etc..Preparation has good
Crystallinity well, high length-diameter ratio, good dispersed and stability hydroxyapatite are always the target that people pursue.
The method of synthesis Oil soluble hydroxy apatite nanometer rods has had wide research at present.CN106835847A is public
The preparation method for having opened a kind of bio-compatibility carbon nanometer tube/hydroxyapatite extrusion coating paper, by CaCl2, NaOH and NaH2PO4·
2H2O three's aqueous solution is added dropwise respectively in the mixed solution of the oleic acid containing carbon nanotube and ethyl alcohol；Mixture is transferred to high pressure
In reaction kettle, reacted 10-20 hours under 190 DEG C of air-proof conditions；It is cooled to room temperature, is washed for several times, obtained with ethyl alcohol and deionized water
Carbon nanometer tube/hydroxyapatite nano wire composite granule.CN105293461A discloses a kind of Oil soluble hydroxy apatite nanometer
The preparation method of piece, by solubility calcium saline solution and low-carbon alcohols, fatty acid and organic amine are added in three-necked flask and mix, stirring
Obtain homogeneous solution；Under agitation, it by soluble phosphoric acid saline solution, is slowly dropped in above-mentioned solution, is added and completes
After continue to stir；After being warming up to 50-90 DEG C of reaction 3-24 hours, cooled to room temperature is centrifugated with supercentrifuge
It to sediment, is washed using dehydrated alcohol and hexamethylene alternating centrifugal, electrolyte and extra fatty acid obtain in removal system
Oil soluble hydroxy apatite nanometer sheet.CN105384158A provides a kind of preparation method of fluorine hydroxyapatite nano shuttle,
In the mixed liquor of oleic acid, oleyl amine and ethyl alcohol, calcium saline solution, phosphate aqueous solution and villiaumite solution is added, at 0 DEG C~30 DEG C
It carries out mineralising and obtains pure fluorine hydroxyapatite nano shuttle.
Although above-mentioned application has been achieved with greater advance in synthetic method, there are still following deficiencies:
1, synthesize the obtained nanocrystal of method of Oil soluble hydroxy apatite crystallinity, pattern, in terms of deposit
It is being short of, it is caused to be unable to fully realize in material application；
2, sodium phosphate solubility is low, and slowly, alkalinity is too strong to cause synthesis technology to take a long time, and product morphology is equal for dissolution
One；
3, synthetic method is mostly undesirable in oily phase dispersion effect.
It is huge by having to the performance of hydroxyapatite-polymer composite nano materials if the above problem can be overcome simultaneously
Promotion, for polymer matrix Hydroxyapatite Nanocomposites biological field application provide stronger support.
Summary of the invention
The purpose of the present invention is analyze in view of the above technology, it is desirable to provide a kind of raw material sources are abundant, low in cost, synthesis
Simple process, easy to implement, product quality is stablized, and morphology controllable is good, the Oil soluble hydroxy apatite nanometer rods of good dispersion
Preparation method.
The implementation of the object of the invention is the method that one-step method prepares Oil soluble hydroxy apatite nanometer rods, feature
Be: specific step is as follows:
1) 0.02mol soluble calcium salt is dissolved in 20 grams of water, obtains solution A；
The soluble calcium salt is calcium nitrate or calcium chloride；
2) 0.01-0.032mol water soluble alkali is dissolved in the mixed liquor of 40 grams of alcoholic solutions and 0.02-0.04mol oleic acid,
Obtain solution B；
The water soluble alkali is ethylenediamine, sodium hydroxide or potassium hydroxide；
The alcoholic solution is ethyl alcohol or propyl alcohol；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the fatty acid and soluble calcium salt is 1:1-2:1；
The molar ratio of the fatty acid and water soluble alkali is 4:1-1:1；
4) 0.012mol soluble phosphate is dissolved in 30 grams of water, obtains solution D；
The soluble phosphate is tertiary sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate
Or potassium dihydrogen phosphate；
5) under agitation, step 4) acquired solution D is slowly dropped in step 3) acquired solution C, after dripping
Continue to stir 20min, obtains suspension；
6) 0.008-0.012mol aqueous slkali is added into suspension obtained by step 5), continues to stir 10min, be mixed
Liquid；
The aqueous slkali is sodium hydroxide or potassium hydroxide solution；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, the hydro-thermal 3-24h at 80 DEG C -180 DEG C, it is natural
Cooling obtains reaction solution；
8) reaction solution obtained by step 7) is centrifugally separating to obtain Oil soluble hydroxy apatite nanometer rods using supercentrifuge
Sediment, three times using dehydrated alcohol and hexamethylene alternating centrifugal washing precipitate, electrolyte and extra rouge in removal system
Fat acid, obtains Oil soluble hydroxy apatite nanometer rods.
Raw material of the present invention is that nontoxic green, abundance is easy to get, is low in cost, and synthesis technology is simple, process repeatability
It is good；Product quality is stable and morphology controllable is good, good dispersion；The neck such as bio-medical material and coating material can be widely used in
Domain.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of hydroxide radical phosphorite nanocrystalline prepared by embodiment 1,
Fig. 2 is the transmission electron microscope picture of hydroxide radical phosphorite nanocrystalline prepared by embodiment 1.
Specific embodiment
The present invention obtains solution A for soluble calcium salt is soluble in water, and water soluble alkali is dissolved in the mixed liquor of alcoholic solution and oleic acid
In obtain solution B；Solution B is added dropwise in three-necked flask, and solution A is slowly added in solution B, stirs to get solution C；Titanium pigment
Hydrochlorate is soluble in water to obtain solution D；Solution D is slowly added dropwise in solution C, stirs to get mixed liquor；The stirring of water soluble alkali solution
It is added dropwise in above-mentioned mixed liquor；Mixed liquor hydro-thermal 3-24h at 80 DEG C -200 DEG C, is cooled to room temperature and obtains reaction solution；Reaction solution centrifugation
Isolated sediment is washed using dehydrated alcohol and hexamethylene alternating centrifugal, obtains Oil soluble hydroxy apatite nanometer rods.
The diameter of prepared Oil soluble hydroxy apatite nanometer rods is 5-20nm, a length of 50-150nm.Oil soluble hydroxy
Apatite nanometer rods can be easy to form the intimate bright of high degree of dispersion in hexamethylene, toluene, styrene organic solvent
Dispersion liquid.
The present invention is described in detail with specific embodiment below.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
1) 0.02mol calcium nitrate is dissolved in 20 grams of water, obtains solution A；
2) 0.032mol ethylenediamine is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.04mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 2:1；
The molar ratio of the oleic acid and ethylenediamine is 5:4.
4) 0.012mol tertiary sodium phosphate is dissolved in 30 grams of water, obtains solution D；
5) under agitation, step 4) acquired solution D is slowly dropped in step 3) acquired solution C, after dripping
Continue to stir 20min, obtains suspension；
6) 0.012mol sodium hydroxide solution is slowly added dropwise in suspension, stirring 10min obtains mixed liquor；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 6 hours at 180 DEG C, to its nature
Cooling obtains reaction solution；
8) reaction solution obtained by step 7) is centrifugally separating to obtain sediment using supercentrifuge, utilizes dehydrated alcohol and ring
Hexane alternating centrifugal washs three times, and electrolyte and extra fatty acid in removal system obtain Oil soluble hydroxy apatite nanometer
Stick.
The X-ray diffractogram of Oil soluble hydroxy phosphorite nanocrystalline obtained by the present embodiment is shown in Fig. 1, it can be seen from figure 1 that this implementation
The Oil soluble hydroxy apatite nanometer rods crystal phase of example preparation is pure ha phase, and no other miscellaneous phases exist, and crystallinity is good.
Transmission electron microscope picture is shown in Fig. 2, from Figure 2 it can be seen that fluorescence hydroxide radical phosphorite nanocrystalline manufactured in the present embodiment is sheet-shaped
Looks, thickness are about 5-20nm, a length of 50-150nm.
Embodiment 2, with embodiment 1, the difference is that,
1) 0.02mol calcium nitrate is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol ethylenediamine is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.02mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1:1；
The molar ratio of the oleic acid and ethylenediamine is 5:4.
4) 0.012mol tertiary sodium phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.008mol sodium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 3 hours at 180 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 3, with embodiment 1, the difference is that,
1) 0.02mol calcium chloride is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol sodium hydroxide is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.02mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1:1；
The molar ratio of the oleic acid and sodium hydroxide is 5:4.
4) 0.012mol sodium dihydrogen phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.008mol potassium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 24 hours at 180 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 4, with embodiment 1, the difference is that,
1) 0.02mol calcium chloride is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol potassium hydroxide is dissolved in the mixed liquor of 40 grams of propyl alcohol and 0.032mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1.6:1；
The molar ratio of the oleic acid and potassium hydroxide is 2:1.
4) 0.012mol tripotassium phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.0104mol sodium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 12 hours at 120 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 5, with embodiment 1, the difference is that,
1) 0.02mol calcium nitrate is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol potassium hydroxide is dissolved in the mixed liquor of 40 grams of propyl alcohol and 0.036mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1.8:1；
The molar ratio of the oleic acid and potassium hydroxide is 2.25:1.
4) 0.012mol disodium hydrogen phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.0112mol sodium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 12 hours at 80 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 6, with embodiment 1, the difference is that,
1) 0.02mol calcium nitrate is dissolved in 20 grams of water, obtains solution A；
2) 0.01mol potassium hydroxide is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.024mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1.2:1；
The molar ratio of the oleic acid and potassium hydroxide is 2.4:1.
4) 0.012mol potassium dihydrogen phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.0088mol potassium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 10 hours at 80 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 7, with embodiment 1, the difference is that,
1) 0.02mol calcium chloride is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol potassium hydroxide is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.04mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 2:1；
The molar ratio of the oleic acid and potassium hydroxide is 2.5:1.
4) 0.012mol potassium dihydrogen phosphate is dissolved in 30 grams of water, obtains solution D；
6) 0.012mol sodium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 20 hours at 80 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 8, with embodiment 1, the difference is that,
1) 0.02mol calcium chloride is dissolved in 20 grams of water, obtains solution A；
2) 0.02mol sodium hydroxide is dissolved in the mixed liquor of 40 grams of propyl alcohol and 0.04mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 2:1；
The molar ratio of the oleic acid and potassium hydroxide is 2:1.
4) 0.012mol dipotassium hydrogen phosphate is dissolved in 30 grams of water, obtains solution D；
5) under agitation, step 4) acquired solution D is slowly dropped in step 3) acquired solution C, after dripping
Continue to stir 20min, obtains suspension E；
6) 0.012mol sodium hydroxide solution is slowly added dropwise in suspension obtained by step 5), stirring 10min is mixed
Close liquid；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 12 hours at 80 DEG C, to its nature
Cooling obtains reaction solution.
Embodiment 9, with embodiment 1, the difference is that,
1) 0.02mol calcium nitrate is dissolved in 20 grams of water, obtains solution A；
2) 0.016mol potassium hydroxide is dissolved in the mixed liquor of 40 grams of ethyl alcohol and 0.02mol oleic acid, obtains solution B；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution
In B, stirs in 10min, obtain solution C；
The molar ratio of the oleic acid and calcium is 1:1；
The molar ratio of the oleic acid and potassium hydroxide is 1.25:1.
4) 0.012mol tripotassium phosphate is dissolved in 30 grams of water, obtains solution D；
5) under agitation, step 4) acquired solution D is slowly dropped in step 3) acquired solution C, after dripping
Continue to stir 20min, obtains suspension；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 24 hours at 80 DEG C, to its nature
Cooling obtains reaction solution.
Claims (2)
1. the method that one-step method prepares Oil soluble hydroxy apatite nanometer rods, it is characterised in that: specific step is as follows:
1) 0.02mol soluble calcium salt is dissolved in 20 grams of water, obtains solution A；
The soluble calcium salt is calcium nitrate or calcium chloride；
2) 0.01-0.032mol water soluble alkali is dissolved in the mixed liquor of 40 grams of alcoholic solutions and 0.02-0.04mol oleic acid, is obtained molten
Liquid B；
The water soluble alkali is ethylenediamine, sodium hydroxide or potassium hydroxide；
The alcoholic solution is ethyl alcohol or propyl alcohol；
3) step 2) acquired solution B is added in three-necked flask, then step 1) acquired solution A is slowly dropped into solution B,
It stirs in 10min, obtains solution C；
The molar ratio of the fatty acid and soluble calcium salt is 1:1-2:1；
The molar ratio of the fatty acid and water soluble alkali is 4:1-1:1；
4) 0.012mol soluble phosphate is dissolved in 30 grams of water, obtains solution D；
The soluble phosphate is tertiary sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate or phosphorus
Acid dihydride potassium；
5) under agitation, step 4) acquired solution D is slowly dropped in step 3) acquired solution C, is continued after dripping
20min is stirred, suspension is obtained；
6) 0.008-0.012mol aqueous slkali is added into suspension obtained by step 5), continues to stir 10min, obtains mixed liquor；
The aqueous slkali is sodium hydroxide or potassium hydroxide solution；
7) mixed liquor obtained by step 6) is placed in high-temperature high-pressure reaction kettle, hydro-thermal 3-24h, natural cooling at 80 DEG C -180 DEG C
Obtain reaction solution；
8) reaction solution obtained by step 7) Oil soluble hydroxy apatite nanometer rods are centrifugally separating to obtain using supercentrifuge to precipitate
Object, three times using dehydrated alcohol and hexamethylene alternating centrifugal washing precipitate, electrolyte and extra fatty acid in removal system,
Obtain Oil soluble hydroxy apatite nanometer rods.
2. the method that one-step method according to claim 1 prepares Oil soluble hydroxy apatite nanometer rods, it is characterised in that: step
It is rapid 8) prepared by Oil soluble hydroxy apatite nanometer rods diameter be 5-20nm, a length of 50-150nm.
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Cited By (4)
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|---|---|---|---|---|
| CN109911874A (en) * | 2019-04-04 | 2019-06-21 | 扬州大学 | A kind of preparation method of the hydroxyapatite of imitative enamel ordered structure |
| CN112300412A (en) * | 2020-11-18 | 2021-02-02 | 重庆大学 | Ionic hydrogel and preparation method thereof |
| CN115154657A (en) * | 2022-07-12 | 2022-10-11 | 山东大学齐鲁医院 | Hydroxyapatite nanorod and application thereof in bone defect repair field |
| CN116374973A (en) * | 2023-02-08 | 2023-07-04 | 浙江大学 | Method for preparing hydroxyapatite with uniformly dispersed aqueous phase by double-layer oleic acid method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109911874A (en) * | 2019-04-04 | 2019-06-21 | 扬州大学 | A kind of preparation method of the hydroxyapatite of imitative enamel ordered structure |
| CN109911874B (en) * | 2019-04-04 | 2022-04-29 | 扬州大学 | Preparation method of hydroxyapatite with imitated enamel ordered structure |
| CN112300412A (en) * | 2020-11-18 | 2021-02-02 | 重庆大学 | Ionic hydrogel and preparation method thereof |
| CN112300412B (en) * | 2020-11-18 | 2021-06-29 | 重庆大学 | Ionic hydrogel and preparation method thereof |
| CN115154657A (en) * | 2022-07-12 | 2022-10-11 | 山东大学齐鲁医院 | Hydroxyapatite nanorod and application thereof in bone defect repair field |
| CN115154657B (en) * | 2022-07-12 | 2023-12-26 | 山东大学齐鲁医院 | Hydroxyapatite nanorod and application thereof in bone defect repair field |
| CN116374973A (en) * | 2023-02-08 | 2023-07-04 | 浙江大学 | Method for preparing hydroxyapatite with uniformly dispersed aqueous phase by double-layer oleic acid method |
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