CN107224606A - A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills - Google Patents
A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills Download PDFInfo
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- CN107224606A CN107224606A CN201710486636.5A CN201710486636A CN107224606A CN 107224606 A CN107224606 A CN 107224606A CN 201710486636 A CN201710486636 A CN 201710486636A CN 107224606 A CN107224606 A CN 107224606A
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- sebacic acid
- alcohol ester
- sills
- pgs
- propyl tri
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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
- A61L27/14—Macromolecular materials
- A61L27/18—Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L27/56—Porous materials, e.g. foams or sponges
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Transplantation (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Dermatology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Materials For Medical Uses (AREA)
Abstract
The present invention relates to a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills, including:Sebacic acid and propyl tri-alcohol ester PGS sills and PLA PLLA is miscible in solvent, mixed solution is configured under the conditions of 50 60 DEG C, is subsequently poured into mould, rear substitution solvent is freezed, freeze-drying obtains nanofibrious scaffold;It is 180~200 DEG C to be subsequently placed in temperature, and air pressure is 24~96h in 100Pa vacuum drying chamber, is produced.Preparation method of the present invention is simple, and various three-dimensional appearances can be made as needed to be adapted to various needs for obtained PGS sill macropores support.
Description
Technical field
The invention belongs to the preparation field of tissue engineering bracket, more particularly to a kind of sebacic acid and propyl tri-alcohol ester PGS base materials
The preparation method of the three-dimensional macropore support of material.
Background technology
Sebacic acid and propyl tri-alcohol ester (PGS) sill is a kind of thermosets, and its prepolymer is viscous at ambient temperature
Thick shape, it is impossible to directly apply to support and prepare, it is necessary to which heat cure is carried out under the hot conditions of anaerobic low pressure could be used for tissue
Engineering rack application, the PGS sills of solidification have good biocompatibility, biodegradable properties and elastic performance.And
It is even more current Research Challenges that PGS sills are prepared into the macropore support with three-dimensional structure, because conventional hole forming technology,
Such as gas foaming method, freeze-drying, it is impossible to which the curing process directly with PGS sills is combined.
The method for being usually used in preparing PGS sill macropore supports at present is salt grain pore method, generally again including two kinds of implementations
Technology.One kind is salt crystallisation, is that supersaturated saline solution is applied into die surface and mould is placed in hot environment, with
The loss of moisture, salt can gradually separate out and form crystal growth in die surface.Its shortcoming is:
(1) in the mould of three-dimensional structure, crystal density heterogeneity, it is difficult to made by way of crystallization between salt grain fully
Contact with each other, thus be difficult to prepare the larger three-dimensional structure support of volume;
(2) salt crystallization is easily caved in during PGS sill solution is irrigated, and preparation process is difficult to accurate control.
Another implementation is to fill up after salt to compress into mould, makes to contact with each other between salt particle, to reach aperture
The purpose of UNICOM, its shortcoming is:
(1) though used in salt grain by grinding, can not ensure that its granular size is homogeneous;
(2) in complex three-dimensional mould is tamped, because unbalance stress causes the Density inhomogeneity of each several part salt.
Because in actual application, tissue engineering bracket often needs that a variety of three-dimensional structures are made, therefore explores
It is a kind of simple to operate, it is with low cost, cell will not be had a negative impact, complex three-dimensional structure PGS base materials can be prepared
The method of material macropore support is particularly important.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of three-dimensional macropore branch of sebacic acid and propyl tri-alcohol ester PGS sills
The preparation method of frame, instant invention overcomes the deficiency of existing sebacic acid and propyl tri-alcohol (PGS) sill macropore support technology of preparing,
A kind of preparation method of the three-dimensional macropore support of PGS sills is obtained, the technology is using PLA (PLLA) as pore-foaming agent, to cell
Have no adverse effect;It can pass through the miscible rear lyophilized re-solidified side of different quality ratio and PGS sills as the PLLA of pore-foaming agent
Formula obtains different porositys;At the same time, the technical operation is simple and convenient.
A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills of the present invention, including:
(1) it is sebacic acid and propyl tri-alcohol ester PGS sills and PLA PLLA is miscible in solvent, under the conditions of 50-60 DEG C
Mixed solution is configured to, is subsequently poured into mould, rear substitution solvent is freezed, freeze-drying obtains nanofibrious scaffold;
(2) it is 180~200 DEG C above-mentioned nanofibrious scaffold to be placed in into temperature, and air pressure is 100Pa vacuum drying chamber
In 24~96h, melt PLLA while solidification PGS sills, produce the three-dimensional macropore of sebacic acid and propyl tri-alcohol ester PGS sills
Support.
Sebacic acid and propyl tri-alcohol ester PGS sills are sebacic acid and propyl tri-alcohol ester PGS, the poly- (last of the ten Heavenly stems two in the step (1)
Acid-
Glycerine-lactic acid-polyethylene glycol-glycerine) one kind in ester PGSLP.
Sebacic acid and propyl tri-alcohol ester PGS sills and PLA PLLA mass ratio are 3 in the step (1):7~7:3.
The concentration of mixed solution is 0.1g/mL in the step (1).
Solvent is one or both of tetrahydrofuran, 1,4- dioxane in the step (1).
Mould is three-dimensional mould in the step (1).
Freezing rear substitution solvent is specially in the step (1):Mixture of ice and water is used after -20~-80 DEG C of 4~24h of freezing
Replace material
In solvent.
Sublimation drying is 0.5-2d in the step (1).
Beneficial effect
(1) the invention provides a kind of preparation strategy of new thermosetting PGS sill macropore supports, and this method is grasped
Make step simple;
(2) present invention is used to make the PLA (PLLA) of PGS sills formation macroporous structure not produce cytotoxicity, and energy
The mechanical strength of reinforcing material, there is application prospect in field of tissue engineering technology;
(3) various three-dimensional appearances can be made PGS sill macropores support prepared by the present invention as needed to be adapted to respectively
Planting needs.
Brief description of the drawings
A, B, C are the SEM pictures of the PGS sill macropore supports prepared in embodiment 1,2,3 respectively in Fig. 1;
Fig. 2 is the exterior appearance of the preceding PGS sills of solidification and PLLA composites in the step of embodiment 2 (1);
Fig. 3 is embodiment 1, the compression stress strain curve of macropore support prepared by embodiment 2 and embodiment 3;
Fig. 4 is embodiment 1, the Young's modulus of macropore support prepared by embodiment 2 and embodiment 3.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester (PGS) sill, key step is as follows:
(1) by sebacic acid and propyl tri-alcohol ester (PGS) and PLA (PLLA) with 3:7 (w/w) are miscible in tetrahydrofuran, and 60
Poured into after the solution that concentration is 10% (w/v) is configured under the conditions of DEG C in a diameter of 2cm, cylindrical three-dimensional mould, be placed in -80
DEG C freezing 4h after with mixture of ice and water replace material in solvent, then freeze-drying obtain nanofibrious scaffold within 2 days;
(2) it is 180 DEG C obtained nanofibrious scaffold in step (1) to be placed in into temperature, and air pressure is 100Pa vacuum
96h in drying box, melts PLLA while solidification PGS sills, obtains with three-dimensional structure, and Young's modulus is 7.04 ±
1.37MPa, aperture is 639.188 ± 196.029 μm of PGS macropore supports.
Embodiment 2
A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester (PGS) sill, key step is as follows:
(1) by poly- (decanedioic acid-glycerine-lactic acid-polyethylene glycol-glycerine) ester (PGSLP) and PLA (PLLA) with 5:5
(w/w) it is miscible in tetrahydrofuran, a diameter of 3cm is poured into after the solution that concentration is 10% (w/v) is configured under the conditions of 60 DEG C, circle
In the three-dimensional mould of cylindricality, the solvent replaced with mixture of ice and water in material is placed in after -20 DEG C of freezing 24h, 2 are then freeze-dried
It obtains nanofibrious scaffold;
(2) it is 190 DEG C obtained nanofibrious scaffold in step (1) to be placed in into temperature, and air pressure is 100Pa vacuum
48h in drying box, melts PLLA while solidification PGS sills, obtains with three-dimensional structure, and Young's modulus is 4.48 ±
1.01MPa, aperture is 282.529 ± 86.927 μm of PGSLP macropore supports.
Embodiment 3
A kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester (PGS) sill, key step is as follows:
(1) by poly- (decanedioic acid-glycerine-lactic acid-polyethylene glycol-glycerine) ester (PGSLP) and PLA (PLLA) with 7:3
(w/w) it is miscible in tetrahydrofuran, a diameter of 4cm is poured into after the solution that concentration is 10% (w/v) is configured under the conditions of 60 DEG C, circle
In the three-dimensional mould of cylindricality, the solvent replaced with mixture of ice and water in material is placed in after -50 DEG C of freezing 12h, 2 are then freeze-dried
It obtains nanofibrious scaffold;
(2) it is 200 DEG C obtained nanofibrious scaffold in step (1) to be placed in into temperature, and air pressure is 100Pa vacuum
24h in drying box, melts PLLA while solidification PGS sills, obtains with three-dimensional structure, and Young's modulus is 2.29 ±
0.26MPa, aperture is 151.610 ± 52.762 μm of PGSLP macropore supports.
Claims (8)
1. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills, including:
(1) it is sebacic acid and propyl tri-alcohol ester PGS sills and PLA PLLA is miscible in solvent, prepared under the conditions of 50-60 DEG C
Into mixed solution, it is subsequently poured into mould, freezes rear substitution solvent, freeze-drying obtains nanofibrious scaffold;
(2) it is 180~200 DEG C above-mentioned nanofibrious scaffold to be placed in into temperature, and air pressure is in 100Pa vacuum drying chamber 24
~96h, produces the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills.
2. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Sebacic acid and propyl tri-alcohol ester PGS sills are sebacic acid and propyl tri-alcohol ester PGS, the poly- (last of the ten Heavenly stems in the step (1)
Diacid-glycerine-lactic acid-polyethylene glycol-glycerine) one kind in ester PGSLP.
3. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Sebacic acid and propyl tri-alcohol ester PGS sills and PLA PLLA mass ratio are 3 in the step (1):7~
7:3。
4. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:The concentration of mixed solution is 10% (w/v) in the step (1).
5. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Solvent is one or both of tetrahydrofuran, 1,4- dioxane in the step (1).
6. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Mould is three-dimensional mould in the step (1).
7. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Freezing rear substitution solvent is specially in the step (1):Mixed after -20~-80 DEG C of 4~24h of freezing with frozen water
Solvent in thing displacement material.
8. a kind of preparation method of the three-dimensional macropore support of sebacic acid and propyl tri-alcohol ester PGS sills according to claim 1,
It is characterized in that:Sublimation drying is 0.5-2d in the step (1).
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CN201710486636.5A CN107224606B (en) | 2017-06-23 | 2017-06-23 | Preparation method of poly-sebacic acid glycerol ester PGS (PGS) -based three-dimensional macroporous scaffold |
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CN201710486636.5A CN107224606B (en) | 2017-06-23 | 2017-06-23 | Preparation method of poly-sebacic acid glycerol ester PGS (PGS) -based three-dimensional macroporous scaffold |
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Cited By (1)
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CN109097910A (en) * | 2018-07-26 | 2018-12-28 | 北京化工大学常州先进材料研究院 | The preparation and application of PGS/ polylactic acid nuclear shell structure nano tunica fibrosa |
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CN102971018A (en) * | 2010-05-11 | 2013-03-13 | 阿勒根公司 | Porogen compositions, methods of making and uses |
CN103201324A (en) * | 2010-05-10 | 2013-07-10 | 阿勒根公司 | Porous materials, methods of making and uses |
WO2014100718A1 (en) * | 2012-12-21 | 2014-06-26 | University Of Pittsburgh - Of The Commonwealth System Of Higher Education | Methods of electrospinning and compositions made therefrom |
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2017
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CN103201324A (en) * | 2010-05-10 | 2013-07-10 | 阿勒根公司 | Porous materials, methods of making and uses |
CN102971018A (en) * | 2010-05-11 | 2013-03-13 | 阿勒根公司 | Porogen compositions, methods of making and uses |
WO2014100718A1 (en) * | 2012-12-21 | 2014-06-26 | University Of Pittsburgh - Of The Commonwealth System Of Higher Education | Methods of electrospinning and compositions made therefrom |
Non-Patent Citations (1)
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CN109097910A (en) * | 2018-07-26 | 2018-12-28 | 北京化工大学常州先进材料研究院 | The preparation and application of PGS/ polylactic acid nuclear shell structure nano tunica fibrosa |
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