CN106540328A - The preparation method of hydroxyapatite polymeric lactic acid compound film - Google Patents
The preparation method of hydroxyapatite polymeric lactic acid compound film Download PDFInfo
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- CN106540328A CN106540328A CN201611052460.4A CN201611052460A CN106540328A CN 106540328 A CN106540328 A CN 106540328A CN 201611052460 A CN201611052460 A CN 201611052460A CN 106540328 A CN106540328 A CN 106540328A
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- hydroxyapatite
- lactic acid
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L27/425—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of phosphorus containing material, e.g. apatite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/40—Preparation and treatment of biological tissue for implantation, e.g. decellularisation, cross-linking
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Abstract
The present invention discloses a kind of preparation method of hydroxyapatite polymeric lactic acid compound film, initially with chemical precipitation method with the CaCl of 0.5mol/L2·2H2O and Na2HPO4Solution prepares hydroxy apatite powder for raw material；Pretreatment is carried out to stainless steel 304；Polylactic acid is dissolved in dichloromethane at room temperature, is stirred, added hydroxy apatite powder stirring 24h, hydroxyapatite polymeric lactic acid compound film is prepared using spin-coating method.The present invention is simple to operate, and the hydroxyapatite polymeric lactic acid compound film purity for preparing is high, degree of crystallinity is high, good mechanical property.
Description
Technical field
The invention belongs to the preparation field of composite, and in particular to a kind of system of hydroxyapatite-polymeric lactic acid compound film
Preparation Method.
Background technology
Hydroxyapatite (hydroxyapatite, HA) molecular formula is Ca10(PO4)6(OH)2, with human body bone-like apatite
The similar the Nomenclature Composition and Structure of Complexes of stone, and with good biocompatibility and activity, implantation human body will not cause rejection, can be with
The very strong chemical bond of people's bone formation, so hydroxyapatite is widely used in hard tissue substituting material.But pure HA is due to mechanics
Poor performance, fragility are big, intensity is relatively low and limit its clinical practice the shortcomings of easy fracture.The bioabsorbable polymer material of synthetic
Polylactic acid (polylactic acid, PLA) with good physicochemical property, mechanical property and processing characteristics, in vivo
Final catabolite is carbon dioxide and water, harmless, be using more Biodegradable material on Medical, but
Be, due to the defect such as hydrophilic and mechanical strength of PLA it is also inadequate separately as bone material.At present, by PLA and HA complexs
Into composite purity it is low, affect its performance.
The content of the invention
For the defect of prior art, the present invention is intended to provide a kind of preparation side of hydroxyapatite-polymeric lactic acid compound film
Method.
The present invention is achieved by the following technical solutions.
The preparation method of hydroxyapatite-polymeric lactic acid compound film, comprises the steps of：
（1）The preparation of hydroxy apatite powder：First, prepare the CaCl of 0.5 mol/L2·2H2O and Na2HPO4Solution, according to
CaCl2·2H2O and Na2HPO4Mol ratio be 5：3, using constant-current titration pump by a certain amount of Na2HPO4With the speed of 2 mL/min
Degree is added drop-wise to the CaCl that mixing speed is 350 r/min2·2H2In O solution, pH=is adjusted with the NaOH solution of 0.5mol/L
10.5, ethanolamine is added, is continued stirring 2h after completion of dropping, is stood 24h, by precipitate with deionized water washing, vacuum filtration, weight
Operate 3 times again, then use absolute ethanol washing sucking filtration, to filtrate pH=7, filter cake is placed in 90 DEG C of drying baker and dries 12 h, obtained
Hydroxyapatite presoma, dry sample Achatess grinding alms bowl are pulverized, and cross 200 mesh sieves, are placed in Muffle furnace calcination, obtain
Hydroxy apatite powder；
（2）Base material pretreatment：Stainless steel 304 is cut into into the cuboid of 10mm × 10mm × 1mm, successively with the SiC water of 220#
Sand papering surface, then by the stainless steel 304 polished successively with acetone, dehydrated alcohol and distilled water in supersonic cleaning machine
Each 10min is cleaned, freeze-day with constant temperature 2h at putting after cleaning 60 DEG C in people's vacuum drying oven；
（3）The preparation of hydroxyapatite-polymeric lactic acid compound film：Weigh 10g polylactic acid and be dissolved in 150mL dichloromethane at room temperature
In, 2h is stirred, step is added（1）The hydroxy apatite powder 100g for obtaining, magnetic agitation 24h under room temperature are existed using spin-coating method
Step（2）Stainless steel surfaces prepare hydroxyapatite-polymeric lactic acid compound film, with spin coating rotational speed 30s of 3000 r/min,
It is then placed in tube furnace, heat treatment 4h, natural cooling obtains hydroxyapatite-polymeric lactic acid compound film.
Preferably, above-mentioned steps（1）The condition of middle Muffle furnace calcination is calcination 2h at 700 DEG C.
Preferably, above-mentioned steps（3）In in tube furnace heat treatment 4h be in 300 DEG C of air atmosphere, air atmosphere 600
DEG C, each at 300 DEG C of nitrogen atmosphere, 600 DEG C of nitrogen atmosphere process 1h.
Advantages of the present invention：
The present invention is simple to operate, and the hydroxyapatite for preparing-polymeric lactic acid compound film purity is high, degree of crystallinity is high, mechanical performance
It is good.
Specific embodiment
Embodiment 1
The preparation method of hydroxyapatite-polymeric lactic acid compound film, comprises the steps of：
（1）The preparation of hydroxy apatite powder：First, prepare the CaCl of 0.5 mol/L2·2H2O and Na2HPO4Solution, according to
CaCl2·2H2O and Na2HPO4Mol ratio be 5：3, using constant-current titration pump by a certain amount of Na2HPO4With the speed of 2 mL/min
Degree is added drop-wise to the CaCl that mixing speed is 350 r/min2·2H2In O solution, pH=is adjusted with the NaOH solution of 0.5mol/L
10.5, ethanolamine is added, is continued stirring 2h after completion of dropping, is stood 24h, by precipitate with deionized water washing, vacuum filtration, weight
Operate 3 times again, then use absolute ethanol washing sucking filtration, to filtrate pH=7, filter cake is placed in 90 DEG C of drying baker and dries 12 h, obtained
Hydroxyapatite presoma, dry sample Achatess grinding alms bowl are pulverized, and cross 200 mesh sieves, are placed in Muffle furnace calcination, obtain
Hydroxy apatite powder；
（2）Base material pretreatment：Stainless steel 304 is cut into into the cuboid of 10mm × 10mm × 1mm, successively with the SiC water of 220#
Sand papering surface, then by the stainless steel 304 polished successively with acetone, dehydrated alcohol and distilled water in supersonic cleaning machine
Each 10min is cleaned, freeze-day with constant temperature 2h at putting after cleaning 60 DEG C in people's vacuum drying oven；
（3）The preparation of hydroxyapatite-polymeric lactic acid compound film：Weigh 10g polylactic acid and be dissolved in 150mL dichloromethane at room temperature
In, 2h is stirred, step is added（1）The hydroxy apatite powder 100g for obtaining, magnetic agitation 24h under room temperature are existed using spin-coating method
Step（2）Stainless steel surfaces prepare hydroxyapatite-polymeric lactic acid compound film, with spin coating rotational speed 30s of 3000 r/min,
It is then placed in tube furnace, heat treatment 4h, natural cooling obtains hydroxyapatite-polymeric lactic acid compound film.
Embodiment 2
The preparation method of hydroxyapatite-polymeric lactic acid compound film, comprises the steps of：
（1）The preparation of hydroxy apatite powder：First, prepare the CaCl of 0.5 mol/L2·2H2O and Na2HPO4Solution, according to
CaCl2·2H2O and Na2HPO4Mol ratio be 5：3, using constant-current titration pump by a certain amount of Na2HPO4With the speed of 2 mL/min
Degree is added drop-wise to the CaCl that mixing speed is 350 r/min2·2H2In O solution, pH=is adjusted with the NaOH solution of 0.5mol/L
10.5, ethanolamine is added, is continued stirring 2h after completion of dropping, is stood 24h, by precipitate with deionized water washing, vacuum filtration, weight
Operate 3 times again, then use absolute ethanol washing sucking filtration, to filtrate pH=7, filter cake is placed in 90 DEG C of drying baker and dries 12 h, obtained
Hydroxyapatite presoma, dry sample Achatess grinding alms bowl are pulverized, and cross 200 mesh sieves, are placed in Muffle furnace calcination, Muffle
The condition of stove calcination is calcination 2h at 700 DEG C, obtains hydroxy apatite powder；
（2）Base material pretreatment：Stainless steel 304 is cut into into the cuboid of 10mm × 10mm × 1mm, successively with the SiC water of 220#
Sand papering surface, then by the stainless steel 304 polished successively with acetone, dehydrated alcohol and distilled water in supersonic cleaning machine
Each 10min is cleaned, freeze-day with constant temperature 2h at putting after cleaning 60 DEG C in people's vacuum drying oven；
（3）The preparation of hydroxyapatite-polymeric lactic acid compound film：Weigh 10g polylactic acid and be dissolved in 150mL dichloromethane at room temperature
In, 2h is stirred, step is added（1）The hydroxy apatite powder 100g for obtaining, magnetic agitation 24h under room temperature are existed using spin-coating method
Step（2）Stainless steel surfaces prepare hydroxyapatite-polymeric lactic acid compound film, with spin coating rotational speed 30s of 3000 r/min,
It is then placed in tube furnace, heat treatment 4h, wherein, in tube furnace, heat treatment 4h is in 300 DEG C of air atmosphere, air atmosphere
600 DEG C, 300 DEG C of nitrogen atmosphere, it is each at 600 DEG C of nitrogen atmosphere process 1h, natural cooling obtains hydroxyapatite-polylactic acid multiple
Close film.
Claims (3)
1. the preparation method of hydroxyapatite-polymeric lactic acid compound film, it is characterised in that：Comprise the steps of：
（1）The preparation of hydroxy apatite powder：First, prepare the CaCl of 0.5 mol/L2·2H2O and Na2HPO4Solution, according to
CaCl2·2H2O and Na2HPO4Mol ratio be 5：3, using constant-current titration pump by a certain amount of Na2HPO4With the speed of 2 mL/min
Degree is added drop-wise to the CaCl that mixing speed is 350 r/min2·2H2In O solution, pH=is adjusted with the NaOH solution of 0.5mol/L
10.5, ethanolamine is added, is continued stirring 2h after completion of dropping, is stood 24h, by precipitate with deionized water washing, vacuum filtration, weight
Operate 3 times again, then use absolute ethanol washing sucking filtration, to filtrate pH=7, filter cake is placed in 90 DEG C of drying baker and dries 12 h, obtained
Hydroxyapatite presoma, dry sample Achatess grinding alms bowl are pulverized, and cross 200 mesh sieves, are placed in Muffle furnace calcination, obtain
Hydroxy apatite powder；
（2）Base material pretreatment：Stainless steel 304 is cut into into the cuboid of 10mm × 10mm × 1mm, successively with the SiC water of 220#
Sand papering surface, then by the stainless steel 304 polished successively with acetone, dehydrated alcohol and distilled water in supersonic cleaning machine
Each 10min is cleaned, freeze-day with constant temperature 2h at putting after cleaning 60 DEG C in people's vacuum drying oven；
（3）The preparation of hydroxyapatite-polymeric lactic acid compound film：Weigh 10g polylactic acid and be dissolved in 150mL dichloromethane at room temperature
In, 2h is stirred, step is added（1）The hydroxy apatite powder 100g for obtaining, magnetic agitation 24h under room temperature are existed using spin-coating method
Step（2）Stainless steel surfaces prepare hydroxyapatite-polymeric lactic acid compound film, with spin coating rotational speed 30s of 3000 r/min,
It is then placed in tube furnace, heat treatment 4h, natural cooling obtains hydroxyapatite-polymeric lactic acid compound film.
2. the preparation method of hydroxyapatite-polymeric lactic acid compound film according to claim 1, it is characterised in that：Step（1）
The condition of middle Muffle furnace calcination is calcination 2h at 700 DEG C.
3. the preparation method of hydroxyapatite-polymeric lactic acid compound film according to claim 1, it is characterised in that：Step（3）
In in tube furnace heat treatment 4h be in 300 DEG C of air atmosphere, 600 DEG C of air atmosphere, 300 DEG C of nitrogen atmosphere, nitrogen atmosphere 600
It is each at DEG C to process 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611052460.4A CN106540328A (en) | 2016-11-25 | 2016-11-25 | The preparation method of hydroxyapatite polymeric lactic acid compound film |
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| CN201611052460.4A CN106540328A (en) | 2016-11-25 | 2016-11-25 | The preparation method of hydroxyapatite polymeric lactic acid compound film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107684638A (en) * | 2017-08-11 | 2018-02-13 | 山东大学 | Two-sided refreshing film of a kind of hydroxyapatite PLA biology and preparation method and application |
| CN108744034A (en) * | 2018-06-20 | 2018-11-06 | 深圳大学 | A kind of preparation method of the hydroxyapatite composite membrane of Ag doping |
-
2016
- 2016-11-25 CN CN201611052460.4A patent/CN106540328A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107684638A (en) * | 2017-08-11 | 2018-02-13 | 山东大学 | Two-sided refreshing film of a kind of hydroxyapatite PLA biology and preparation method and application |
| CN108744034A (en) * | 2018-06-20 | 2018-11-06 | 深圳大学 | A kind of preparation method of the hydroxyapatite composite membrane of Ag doping |
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Application publication date: 20170329 |