CN100446817C - Microwave heating process for preparing tissue carrier material of polycaprolactone - Google Patents
Microwave heating process for preparing tissue carrier material of polycaprolactone Download PDFInfo
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- CN100446817C CN100446817C CNB2006100241272A CN200610024127A CN100446817C CN 100446817 C CN100446817 C CN 100446817C CN B2006100241272 A CNB2006100241272 A CN B2006100241272A CN 200610024127 A CN200610024127 A CN 200610024127A CN 100446817 C CN100446817 C CN 100446817C
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Abstract
The present invention discloses a microwave heating process for preparing a tissue carrier material of polycaprolactone, which comprises the following steps: polycaprolactone fiber is cut in length of 1 to 20 and is filled in a mould in the specific shape, the filling quality is evaluated by the porosity of 60 to 95%, and the fiber is arrayed into a uniform structure; the mould is put in a microwave oven at mild fire-middle fire to melt and combine for 1 second to 10 min, the mould is taken out and cooled to the environment temperature, demoulding is done, vacuum drying is carried out for 24 h, and a tissue carrier material of polycaprolactone is prepared. The heat conduction of the present invention is uniform, the good mechanical performance and the higher porosity are provided while the carrier material is formed in one step, and the technological process is simple and is easy to control. Therefore, the present invention can meet clinic requirements of various tissues such as bone, cartilage, etc.
Description
Technical field
The present invention relates to the preparation method fiber of a kind of polycaprolactone (PCL) tissue carrier material, particularly relate to a kind of method for preparing the polycaprolactone tissue carrier material with microwave heating method.
Background technology
Ideal engineering carrier should possess following several functions: [Hutmacher D W.[J] .Biomaterials, 2000,21:2529～2543.] (1) carrier should be three-dimensional, porous network structure, the size in hole should be able to allow the existence of cell, and should connect mutually between the hole, be beneficial to nutrient substance and the transmission of cellular metabolism refuse; (2) excellent biological compatibility and biodegradable, degradation rate should be able to mate with neoblastic growth phase; (3) surface should be suitable for cell adhesion and normal differentiation and propagation; (4) have certain biomechanical property, consistent with the institute repair tissue; (5) can carry active substance.
Rebuild in the research of repair tissue in organizational project, carrier material is the guide.Studies show that the shape of carrier mesopore, size and porosity directly affect migration, differentiation and the propagation of repopulating cell, then great changes have taken place with the difference of preparation method for these factors, and crudy is directly connected to the quality of new organization function.At present, the method for preparing porous carrier materials is varied, and pluses and minuses are respectively arranged, and comprises fiber bonding method, solvent cast-particle leaching method, gas pore method, chemical blowing process, sintering microsphere method, lyophilization and 3 D-printing technology etc.
Organizational project is brand-new research field in recent years, thereby it is also few in number to be relevant to the document and the patent report of preparation aspect of tissue carrier material both at home and abroad.Literature search is found: had some to be used to prepare the report of tissue carrier material for PCL in recent years abroad, but preparation method is had nothing in common with each other, for example human sucrose such as S.-J.Shieh prepares shape template, then in conjunction with solvent cast/particle leaching method, make the cartilage tissue engineered carrier material of ear shape PCL and PHB material, and studied it at the intravital biological nature of nude mice [Shy-Jou Shieh, Schinichi Terada, Joseph P.Vacanti.Tissueengineering auricular reconstruction:in vitro and in vivo studies.Biomaterials 25 (2004) 1545-1557.]; People such as Teoh adopt PCL or PCL/HA filament fiber, by a kind of rapid shaping technique---and fusion sediment method (FDM) preparation three-dimension porous tissue engineering carrier material is used for bone and cartilage tissue engineered [Teoh, Swee Hin, Hutmacher, Dietmar Werner, Tan, Kim Cheng, Tam, Kock Fye, Zein, Iwan.Methods for fabricating afilament for use in tissue engineering.USP-6,730,252.May 4,2004.].And the domestic patent report that does not prepare relevant for the PCL carrier material at present, aspect preparation method, be to prepare bone and cartilage tissue engineered rack material by freeze-drying by collagen/chitosan/GPSM/ lime nitrate intermingling material as: " a kind of three-dimensional porous tissue engineering bracket material and preparation method thereof " of people such as Ren Lei [Chinese patent application number 200410094895.6, publication number CN1613514A]; People's such as Dai Gang " a kind of cartilage tissue engineering scaffold composite material " [Chinese patent application number 02113378.6, publication number CN1380113A] with polylactic acid solution and calcium polyphosphate fiber compound after, adopt founding granule leaching to prepare the bone tissue engineer composite carrier.These researchs mainly are based on some traditional methods and make composite carrier.Obviously, employing PCL is a biomaterial, and the method that the microwave thermal clinkering technology by fiber prepares tissue carrier material does not have similar or similar patent report both at home and abroad.At present, the defective of existing technology of preparing mainly is present in: in the biomaterial of wide selection, natural polymer such as collagen, chitosan etc. lack certain mechanical strength and interior spatial structure, and synthetic high polymer PGA and PLA etc. are prone to the aseptic inflammation reaction because degradation speed is too fast after the degraded; The carrier aperture that makes as freeze-drying in traditional preparation method is less than normal, solvent cast/carrier material that the particle leaching method makes can not satisfy the requirement of high porosity, and many methods need the participation of organic solvent in preparation process, need come common implementing in conjunction with several different methods usually when the complex-shaped carrier material of preparation; And the method for new development such as 3 D-printing technology etc. mainly depend on the support of computer technology.
Summary of the invention
Technical problem to be solved by this invention provides and a kind ofly prepares the method for polycaprolactone tissue carrier material with microwave heating method, to remedy the deficiencies in the prior art or defective, satisfies and produces and the needs of life and the development of some field.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind ofly prepare the method for polycaprolactone tissue carrier material with microwave heating method, comprise the steps:
A, the polycaprolactone fiber is cut into length is 1～20mm, is filled in the mould of given shape, and filling quality is 60%～95% to calculate with porosity, and fiber alignment becomes homogeneous texture;
B, mould heating intensity in microwave oven is adopted warm fire～moderate heat heating clinkering 1 second～10 minutes, take out and be cooled to the demoulding after the ambient temperature, vacuum drying 24 hours promptly makes polycaprolactone organizational project porous carrier materials.
As optimized technical scheme: the molecular weight of described polycaprolactone is 1～200,000, and fusing point is 55～65 ℃; The diameter of described polycaprolactone fiber is 10～500 μ m; The aperture of prepared carrier material is 1～500 μ m.
Even, the three-dimensional connectivity of the prepared PCL porous carrier materials of the present invention internal pore structure is good, the aperture can be at 1～500 μ m, porosity is 60～95% variations, to be ready for use on organizational project after three-dimensional porous carrier material sterilization, the packing, its profile can be some certain organs shapes, is specially adapted to the application of bone or cartilage tissue engineered carrier material.
The invention has the beneficial effects as follows: adopt microwave heating process, make the fiber framework in the clinkering process, inside and outsidely obtained equal heat simultaneously, the inhomogeneities of having avoided heat transfer process to cause to material structure.This method can guarantee that also carrier material is reaching the one-time formed while, possess good mechanical performance and higher porosity, the degradation speed that possesses excellent biological compatibility, controllable adjustment simultaneously owing to PCL, thereby the clinical needs of multiple organizational projects such as applicable bone, cartilage.In addition, the present invention can be fully not with an organic solvent in preparation process, and the easy easy control of technical process, and the characteristics that are better than other many preparation methoies are arranged.Key problem in technology of the present invention is to the accurate selection of microwave radiation amount under the different condition.
Description of drawings
Fig. 1 is the scanning electron microscope picture of polycaprolactone (PCL) tissue carrier material
The specific embodiment
Below in conjunction with specific embodiment the present invention is further elaborated.With reference to accompanying drawing 1
Embodiment 1
With average diameter be that 500 μ m, molecular weight are 10,000, fusing point is that 55 ℃ PCL fiber is cut into the isometric 6.0mm that is, be filled in the mould of given shape, filling quality is 80% calculating with porosity, microwave oven heating shelves are set at " temperature fire ", die sealing is placed in the microwave oven heating clinkering and takes out after 10 minutes, the room temperature cooling back demoulding, vacuum drying just obtained having the tissue carrier material of given configuration and superperformance after 24 hours.It is 300-500 μ m that material records the aperture through scanning electron microscope, and recording porosity by liquid displacement technique is 78%, and hole perforation degree reaches more than 90%, good mechanical performance, and the external degradation cycle is longer.This material is applicable to the bone tissue engineer carrier material, as the repair and reconstruction of bone injury.
Embodiment 2
With average diameter is that (molecular weight is 200,000 for the PCL fiber of 250 μ m, fusing point is 62～65 ℃) be cut into isometric 1.0mm after, be filled in the mould of given shape, filling quality is 95% calculating with porosity, microwave oven heating shelves are set at " low fire ", die sealing is placed in the microwave oven heating clinkering and takes out the demoulding after the room temperature cooling after 3 minutes, behind the vacuum drying 24 hours, just obtain having the tissue carrier material of given configuration and superperformance.Recording the material aperture is 150-300 μ m, and porosity is 94%, and the external degradation cycle is longer, has excellent biological compatibility and mechanical property.This material possesses higher porosity, is particularly useful for cartilage tissue engineered carrier material, can induce chondrocyte to stick preferably and growth, reaches the purpose of repairing the cartilaginous tissue damage.
Embodiment 3
With average diameter is that (molecular weight is 80,000 for the PCL fiber of 10 μ m, fusing point is 58～60 ℃) be cut into isometric 20.0mm after, be filled in the mould of given shape, filling quality is 60% calculating with porosity, microwave oven heating shelves are set at " moderate heat ", and die sealing is placed in the microwave oven heating clinkering and takes out the demoulding after the room temperature cooling after 1 second, behind the vacuum drying 24 hours, just obtain having the tissue carrier material of given configuration and superperformance.Recording the material aperture is 1-150 μ m, and porosity is 65%, and preliminary in vitro tests shows that biological activity and degradation characteristic are good.This material possesses superior mechanical property and suitable degradation cycle, also is applicable to the bone tissue engineer carrier material, and has the effect of induced osteogenesis.
Claims (4)
1, a kind ofly prepares the method for polycaprolactone tissue carrier material, it is characterized in that comprising the steps: with microwave heating method
A, the polycaprolactone fiber is cut into length is 1～20mm, is filled in the mould of given shape, and filling quality is 60%～95% to calculate with porosity, and fiber alignment becomes homogeneous texture;
B, mould heating intensity in microwave oven is adopted warm fire～moderate heat heating clinkering 1 second～10 minutes, take out and be cooled to the demoulding after the ambient temperature, vacuum drying 24 hours promptly makes polycaprolactone organizational project porous carrier materials.
2, method according to claim 1 is characterized in that: the molecular weight of described polycaprolactone is 1～200,000, and fusing point is 55～65 ℃.
3, method according to claim 1 is characterized in that: the diameter of described polycaprolactone fiber is 10～500 μ m.
4, method according to claim 1 is characterized in that: the aperture of prepared carrier material is 1～500 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100241272A CN100446817C (en) | 2006-02-24 | 2006-02-24 | Microwave heating process for preparing tissue carrier material of polycaprolactone |
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| CNB2006100241272A CN100446817C (en) | 2006-02-24 | 2006-02-24 | Microwave heating process for preparing tissue carrier material of polycaprolactone |
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| CN100446817C true CN100446817C (en) | 2008-12-31 |
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| CN106399736B (en) * | 2016-06-28 | 2018-06-12 | 廖川金 | A kind of preparation method of the uniform celled foam aluminium of high density |
| CN113559330B (en) * | 2021-06-18 | 2022-04-29 | 东华大学 | Preparation method of low-filling-amount and highly-orderly-arranged HA-based composite resin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6626950B2 (en) * | 2001-06-28 | 2003-09-30 | Ethicon, Inc. | Composite scaffold with post anchor for the repair and regeneration of tissue |
| JP2004123810A (en) * | 2002-09-30 | 2004-04-22 | Kanebo Ltd | Biodegradable foam and its volume reduction method |
| CN1587294A (en) * | 2004-07-13 | 2005-03-02 | 清华大学 | Process for preparing medical polyurethane and modeling product under single mold microwave radiation |
| CN1593674A (en) * | 2004-06-24 | 2005-03-16 | 上海交通大学 | Biodegradable poly-caprolactone artificial breast wall material and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6626950B2 (en) * | 2001-06-28 | 2003-09-30 | Ethicon, Inc. | Composite scaffold with post anchor for the repair and regeneration of tissue |
| JP2004123810A (en) * | 2002-09-30 | 2004-04-22 | Kanebo Ltd | Biodegradable foam and its volume reduction method |
| CN1593674A (en) * | 2004-06-24 | 2005-03-16 | 上海交通大学 | Biodegradable poly-caprolactone artificial breast wall material and preparation method thereof |
| CN1587294A (en) * | 2004-07-13 | 2005-03-02 | 清华大学 | Process for preparing medical polyurethane and modeling product under single mold microwave radiation |
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