CN107412886A - A kind of preparation method of the biomaterial of sclerosed collagen composite polylactic acid - Google Patents
A kind of preparation method of the biomaterial of sclerosed collagen composite polylactic acid Download PDFInfo
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- CN107412886A CN107412886A CN201710651603.1A CN201710651603A CN107412886A CN 107412886 A CN107412886 A CN 107412886A CN 201710651603 A CN201710651603 A CN 201710651603A CN 107412886 A CN107412886 A CN 107412886A
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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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/041—Mixtures of macromolecular compounds
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/06—At least partially resorbable materials
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/06—At least partially resorbable materials
- A61L17/10—At least partially resorbable materials containing macromolecular materials
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/06—At least partially resorbable materials
- A61L17/10—At least partially resorbable materials containing macromolecular materials
- A61L17/12—Homopolymers or copolymers of glycolic acid or 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/148—Materials at least partially resorbable by the body
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Abstract
The invention discloses a kind of preparation method of the biomaterial of sclerosed collagen composite polylactic acid.In gnotobasis, collagen is weighed, is made 0.1% ~ 25%（W/V）Dispersion liquid, PH scopes 4 ~ 8；Press collagen：Chitosan is（1~100）:（100~1）（W/W）Ratio weigh chitosan, be made 0.1% ~ 10%（W/V）Suspension, PH scopes 2 ~ 8.It is well mixed.Room temperature dehydration, ultraviolet-crosslinkable is to drying, 250 ~ 280nm of irradiation wavelengths when dehydration rate reaches 50% 95%；Last mechanical or manual shaping.PLA is weighed, is pressed with the aqueous slkali that concentration is 0.01 ~ 2.0mol/L（1~100）:（100~1）（W/V）, drying is filtered out after soaking and washing under 25 DEG C ~ 45 DEG C environment, extreme trace cleaning fluid PH is 5 ~ 9；Dried PLA is heated and softened or organic solvent dissolves, the sample surfaces in shaping is then coated with, dries, coat drying repeatedly, it is final to obtain the Biocomposite material for meeting requirement.The material prepared using the present invention is degradable, and degradation speed is controllable, there is certain toughness, is adapted to clinical Various Tissues injury repair treatment.
Description
Technical field
The present invention relates to biology medical material technical field, more particularly to a kind of neutral proteinase extracts glue from ox heel string
Former method.
Background technology
For clinical operation method as the development of science and technology becomes more hommization, particularly wound is more severe at present
Tissue, such as bone split, the fixation of Cranial defect, tissue apposition etc., it is mostly to avoid carrying out second operation to solve direction, in order to avoid to patient
Carry out secondary insult.But different tissue repair time is different, the degradable material of present metal and part is mostly in fixed body
Degradation time, without suspected of a kind of foreign matter for the tissue quickly repaired, internal size is kept for a long time and influence be present.Therefore need
A kind of degradable, controllable degradation speed meets that clinical patients use for the composite of different tissues reparation.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation side of the biomaterial of sclerosed collagen composite polylactic acid
Method, in the case of the complete triple helix structure of collagen can be ensured, hardening shaping collagen, according to PLA different molecular weight
Degradation speed completes the biomaterial of controllable degradation speed jointly.Technical scheme is as follows：
The invention provides a kind of preparation method of the biomaterial of sclerosed collagen composite polylactic acid, comprise the following steps,
（1）The preparation of collagen hardened forming sample
By self-control or the commercially available collagen with triple-helix structure, purified water is dispersed or acid solution dissolves collagen or aqueous slkali is molten
Collagen is solved, is made into 1% ~ 25%（W/V）Collagen dispersion liquid, last acid solution or aqueous slkali adjust PH to 4 ~ 8；
Press collagen：Chitosan is（1~100）:（100~1）（W/W）Ratio weigh chitosan, be configured to 0.1% ~ 10%（W/V）Shell
Glycan suspension, suspension PH are 2 ~ 8；
Chitosan suspension and Collagen dispersions system are mixed evenly, are put into micropore mold, room temperature natural-dehydration is extremely de-
When water rate is 50% ~ 95%, ultraviolet cross-linking radiation to sample drying hardens, 250 ~ 280nm of irradiation wavelengths；
Last mechanical or manual machine-shaping, in drier, room temperature storage is standby；
（2）Self-control or commercially available different molecular weight be 200 ~ 1000000 PLA liquefaction；
The PLA of different molecular weight ranges is heated into 40 DEG C ~ 150 DEG C softening to flowable or organic solvents to be dissolved into
It is liquid.Biometrics technology process often heats up 3 ~ 5 DEG C, need to be incubated 5 ~ 10min.
The PLA of different molecular weight ranges is coated uniformly on the surface of collagen hardening profiles after liquefaction is handled, and vacuum is done
It is dry, coat, dry again again, after repeated multiple times, obtain the biological material for the sclerosed collagen composite polylactic acid for meeting requirement
Material.
In the present invention（1）A kind of preferred embodiment in, collagen decentralized system concentration be 1% ~ 25%（W/V）；
In the present invention（1）A kind of preferred embodiment in, collagen disperse acid solution used for hydrochloric acid solution, phosphoric acid solution,
The one or more of acetic acid solution, citric acid solution.
In the present invention（1）A kind of preferred embodiment in, collagen disperses aqueous slkali used for sodium hydroxide solution, carbon
Sour hydrogen sodium solution, the one or more of sodium citrate solution.
In the present invention（1）A kind of preferred embodiment in, the pH value of Collagen dispersions system is 4 ~ 8.
In the present invention（1）A kind of preferred embodiment in, chitosan property is the water-soluble and molten one or more of acid.
In the present invention（1）A kind of preferred embodiment in, the concentration of chitosan suspension is 0.1% ~ 10%（W/V）.
In the present invention（1）A kind of preferred embodiment in, the pH value of chitosan suspension is 2 ~ 8.
In the present invention（1）A kind of preferred embodiment in, collagen：Chitosan is（1~100）:（100~1）（W/W）.
In the present invention（1）A kind of preferred embodiment in, collagen-chitosan mixed system dry for ultraviolet irradiation it is natural
Dry.250 ~ 280nm of irradiation wavelengths.
In the present invention（1）A kind of preferred embodiment in, the molding mode of collagen hardened blank is laser ablation, lathe
One or more of mechanical-moulded modes in cutting, stamping of powder, cold rolling, calendering, or hand engraving, polishing, cutting, hollow out
In one or more of offhand modes.
In the present invention（2）A kind of preferred embodiment in, self-control or commercially available polylactic acid molecule amount scope be 200 ~
1000000, during the temperature elevating range is 40 ~ 150 DEG C, often heats up 3 ~ 5 DEG C, 5 ~ 10min need to be incubated；
In the present invention（2）A kind of preferred embodiment in, organic solvent be acetone, tetrahydrofuran, dioxane, in chloroform
It is one or more of.
In the present invention（2）A kind of preferred embodiment in, the PLA solution concentration of formation is 1% ~ 100%（W/V）.
In the present invention（2）A kind of preferred embodiment in, collagen hardening profiles surface coating liquefaction PLA method
To impregnate, brushing, high pressure airless spray, electrostatic spraying, the one or more in spin coating.It is specifically used according to product to coat number
Depending on it is required that, usually 2 ~ 8 times.
In the present invention（2）A kind of preferred embodiment in, vacuum drying can be carried out in vacuum drying chamber, and temperature is poly-
Lactic acid softening temperature ± 10 DEG C, first it can also be freezed with after dry ice or liquid nitrogen frozen with freeze dryer.
Embodiment
It should be noted that water used in the present invention is the purified water or water for injection used in pharmaceuticals industry, meet
Standards of pharmacopoeia.
Reagent and instrument
Reagent is commercially available.
Embodiment 1
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, manual kneading is uniform, and Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, injection into strips, is placed on crosslinking with radiation under uviol lamp（Irradiate ripple
Long 270nm）, obtain collagen hardened sample.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C, it is white to obtain 22g
Color solid.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, is heated to 70 DEG C, mechanical agitation to PLA is changed into high viscosity glue
Melt, melt is uniformly applied to strip hardening Collagen specimens surface, sample, which is put into drier, is cooled to room temperature, with liquid nitrogen-
70 DEG C of freezings obtain PLA-collagen composite materials after being freezed in freeze dryer.
Embodiment 2
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, stirred, Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, is put into square dies, is molded into bulk, is placed under uviol lamp
Crosslinking with radiation（Irradiation wavelengths 260nm）, obtain collagen hardened sample.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C, it is white to obtain 20g
Color solid.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, is heated to 70 DEG C, mechanical agitation to PLA is changed into high viscosity glue
Melt, melt is uniformly applied to block sclerosed collagen sample surfaces, sample, which is put into drier, is cooled to room temperature, with liquid nitrogen-
70 DEG C of freezings obtain PLA-collagen composite materials after being freezed in freeze dryer.
Embodiment 3
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, stirred, Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, with mold injection circlewise sample.It is UV-crosslinked（Irradiation wavelengths
280nm）Drying and moulding.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C, it is white to obtain 24g
Color solid.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 65 ~ 75
℃。
（4）The dried PLA of 10g alkali cleanings is taken, is heated to 75 DEG C, mechanical agitation to PLA is changed into high viscosity glue
Melt, melt is uniformly applied to annular sclerosis Collagen specimens surface, sample, which is put into drier, is cooled to room temperature, with liquid nitrogen-
70 DEG C of freezings obtain PLA-collagen composite materials after being freezed in freeze dryer.
Embodiment 4
（1）In desinfection chamber：
The collagen of 29.96g psychrometric ratios 33.37% is weighed, adds 80ml moisture to dissipate, stands 5h；
3.4g chitosans are weighed, are dissolved in 44ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, smashed to pieces to uniform, Room-temperature seal placement 48h；
Mixed collagen is placed in micropore mold and drained away the water, it is UV-crosslinked（Irradiation wavelengths 250nm）Drying is blocking, every piece
0.5g, each fritter are laser machined into screw.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C, it is white to obtain 22g
Color solid.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, is dissolved in 20ml acetone-chloroforms（1:1, v/v）In the mixed solvent, will
The collagen screw specimens of hardening are quickly immersed in above-mentioned solution, pull out after 40 DEG C of solvent removed by vacuum, by gained sample again
In secondary immersion solution, repeat to operate above, after 5 dipping-desolventizings, with -70 DEG C of freezings of liquid nitrogen after being freezed in freeze dryer, obtain
Obtain PLA-collagen composite materials.
Embodiment 5
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22 ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, smashed to pieces to uniform, Room-temperature seal placement 48h；
Mixed collagen is placed in micropore mold and drained away the water, bulk, ultraviolet irradiation are molded into by SLS process moulds（Irradiation
Wavelength 260nm）Collagen hardened sample.（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes PLA sample
24 grams of product, which shred, to be immersed in the sodium bicarbonate solution that 100ml is prepared, and 45 DEG C of stirring 10min, is filtered out solid, is again dipped into
In 100ml alkali lye, 10 min are stirred, so repeatedly 16 times, now surface of solids PH is 6, and washing lotion PH is 7, by solid in 45 DEG C
12h is dried in vacuo, obtains 22g white solids.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 65 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, is dissolved in 20ml acetone-chloroforms（1:1, v/v）In the mixed solvent, will
The block Collagen specimens of hardening are quickly immersed in above-mentioned solution, pull out after 40 DEG C of solvent removed by vacuum, by gained sample again
Immerse in solution, repeat to operate above, after 5 dipping-desolventizings, with -70 DEG C of freezings of liquid nitrogen after being freezed in freeze dryer, obtain
PLA-collagen composite materials.
Embodiment 6
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, manual kneading is uniform, and Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, mold injection is into bulk, ultraviolet irradiation（Irradiation wavelengths 260nm）
Collagen hardened sample.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, 10 mg hexane diisocyanates, is dissolved in 20ml tetrahydrofurans,
The block Collagen specimens of hardening are quickly immersed in above-mentioned solution, pulled out after 35 DEG C of solvent removed by vacuum, by gained sample again
In secondary immersion solution, repeat to operate above, after 5 dipping-desolventizings, be put into solidification 12h in 50 DEG C of vacuum drying chambers, gathered
Lactic acid-collagen composite materials.
Embodiment 7
（1）In desinfection chamber：
The collagen of 29.96g psychrometric ratios 33.37% is weighed, adds 80ml moisture to dissipate, stands 5h；
3.4g chitosans are weighed, are dissolved in 44ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, manual kneading is uniform, and Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, it is UV-crosslinked（Irradiation wavelengths 275nm）Drying is blocking, every piece
0.5g, each fritter are laser machined into screw.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, 10 mg hexane diisocyanates, is dissolved in 20ml tetrahydrofurans,
The collagen screw specimens of hardening are quickly immersed in above-mentioned solution, pulled out after 35 DEG C of solvent removed by vacuum, by gained sample
It is again dipped into solution, repeats to operate above, after 5 dipping-desolventizings, is put into solidification 12h in 50 DEG C of vacuum drying chambers, obtains
PLA-collagen composite materials.
Embodiment 8
（1）In desinfection chamber：
The collagen of 14.98g psychrometric ratios 33.37% is weighed, adds 40ml moisture to dissipate, stands 2h；
1.7g chitosans are weighed, are dissolved in 22ml 0.1mol/L hydrochloric acid；
Chitosan salt acid solution is poured into collagen dispersion, stirred, Room-temperature seal places 48h；
Mixed collagen is placed in micropore mold and drained away the water, mold injection is UV-crosslinked（Irradiation wavelengths 260nm）It is dried to
Strip.
（2）Compound concentration is the 0.01mol/L ml of sodium bicarbonate solution 2000, takes 24 grams of PLA sample to shred immersion
In the sodium bicarbonate solution that 100ml is prepared, 45 DEG C of stirring 10min, solid is filtered out, is again dipped into 100ml alkali lye, stirring 10
Min, so repeatedly 15 times, now surface of solids PH is 5, and washing lotion PH is 7, and solid is dried in vacuo into 12h in 45 DEG C.
（3）The PLA solid that 10g is dried is taken, shreds and is put into 50ml beakers, be placed in water bath with thermostatic control, initial temperature
30 DEG C of degree, 1 DEG C/min of heating rate, every liter 5 DEG C, soaking time 5min, the softening range for measuring PLA is 60 ~ 70
℃。
（4）The dried PLA of 10g alkali cleanings is taken, 10 mg hexane diisocyanates, is dissolved in 20ml tetrahydrofurans,
The strip Collagen specimens of hardening are quickly immersed in above-mentioned solution, pulled out after 35 DEG C of solvent removed by vacuum, by gained sample again
In secondary immersion solution, repeat to operate above, after 5 dipping-desolventizings, be put into solidification 12h in 50 DEG C of vacuum drying chambers, gathered
Lactic acid-collagen composite materials.
It is described above to be for only for ease of it will be understood by those skilled in the art that technical scheme, not limiting
The present invention.Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in this
Within the protection domain of invention.
Claims (9)
- A kind of 1. preparation method of the biomaterial of sclerosed collagen composite polylactic acid, it is characterised in that comprise the following steps,（1）The preparation of collagen hardened forming sampleBy self-control or the commercially available collagen with triple-helix structure, purified water is dispersed or acid solution dissolves collagen or aqueous slkali is molten Collagen is solved, is made into 1% ~ 25%（W/V）Collagen dispersion liquid, last acid solution or aqueous slkali adjust PH to 4 ~ 8；Press collagen：Chitosan is（1~100）:（100~1）（W/W）Ratio weigh chitosan, be configured to 0.1% ~ 10%（W/V）Shell Glycan suspension, suspension PH are 2 ~ 8；Chitosan suspension and Collagen dispersions system are mixed evenly, are put into micropore mold, room temperature natural-dehydration is extremely de- When water rate is 50% ~ 95%, ultraviolet cross-linking radiation to sample drying hardens, 250 ~ 280nm of irradiation wavelengths；Last mechanical or manual machine-shaping, in drier, room temperature storage is standby；（2）Self-control or commercially available different molecular weight be 200 ~ 1000000 PLA liquefaction；The PLA of different molecular weight ranges is heated into 40 DEG C ~ 150 DEG C softening to flowable or organic solvents to be dissolved into It is liquid；Biometrics technology process often heats up 3 ~ 5 DEG C, need to be incubated 5 ~ 10min；The PLA of different molecular weight ranges is coated uniformly on the surface of collagen hardening profiles after liquefaction is handled, vacuum drying, Coat, dry again again, after repeated multiple times, obtain the biomaterial for the sclerosed collagen composite polylactic acid for meeting requirement.
- 2. according to claim 1（1）Described method, it is characterised in that the collagen decentralized system concentration is 1% ~ 25%（W/ V）；The collagen disperses acid solution used for hydrochloric acid solution, phosphoric acid solution, acetic acid solution, one kind or several of citric acid solution Kind；The collagen disperses aqueous slkali used for sodium hydroxide solution, sodium bicarbonate solution, one kind or several of sodium citrate solution Kind；The chitosan property is one or more water-soluble and that acid is molten.
- 3. according to claim 1（1）Described method, it is characterised in that the pH value of the Collagen dispersions system is 4 ~ 8；The shell The concentration of glycan suspension is 0.1% ~ 10%（W/V）；The pH value of the chitosan suspension is 2 ~ 8；The collagen：Chitosan is （1~100）:（100~1）（W/W）；The collagen-chitosan mixed system is dried to be spontaneously dried for ultraviolet irradiation, irradiation wavelengths 250 ~280nm。
- 4. according to claim 1（1）Described method, it is characterised in that the molding mode of the collagen hardened blank is laser One or more of mechanical-moulded modes in ablation, machine cut, stamping of powder, cold rolling, calendering, or hand engraving, polishing, One or more of offhand modes in cutting, hollow out.
- 5. according to claim 1（2）Described method, it is characterised in that self-control or commercially available polylactic acid molecule amount scope be 200 ~ 1000000, during the temperature elevating range is 40-150 DEG C, often heats up 3 ~ 5 DEG C, 5 ~ 10min need to be incubated.
- 6. according to claim 1（2）Described method, it is characterised in that the organic solvent is acetone, tetrahydrofuran, dioxy One or more in six rings, chloroform.
- 7. according to claim 1（2）Described method, it is characterised in that the PLA solution concentration of the formation is 1% ~ 100% （W/V）.
- 8. according to claim 1（2）Described method, it is characterised in that the poly- breast of collagen hardening profiles surface coating liquefaction The method of acid is the one or more in dipping, brushing, high pressure airless spray, electrostatic spraying, spin coating.Number is coated according to product Depending on specifically used requirement, usually 2 ~ 8 times.
- 9. according to claim 1（2）Described method, it is characterised in that described vacuum drying can enter in vacuum drying chamber OK, temperature is PLA softening temperature ± 10 DEG C, first can also be freezed with after dry ice or liquid nitrogen frozen with freeze dryer.
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