CN109381747A - A kind of preparation method of polylactic acid-chitose fiber scaffold material - Google Patents
A kind of preparation method of polylactic acid-chitose fiber scaffold material Download PDFInfo
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- CN109381747A CN109381747A CN201710681147.5A CN201710681147A CN109381747A CN 109381747 A CN109381747 A CN 109381747A CN 201710681147 A CN201710681147 A CN 201710681147A CN 109381747 A CN109381747 A CN 109381747A
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- polylactic acid
- chitose
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- preparation
- chitosan
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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
- 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
- A61L27/14—Macromolecular materials
- A61L27/20—Polysaccharides
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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
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- 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)
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Abstract
The invention discloses a kind of preparation methods of polylactic acid-chitose fiber scaffold material, comprising: (1) prepares PLA solution: acetone soln is added in polylactic acid, 60~90min of magnetic agitation obtains PLA solution；(2) it prepares chitosan solution: chitosan is added to the water, stir 10~20min, obtain chitosan solution；It (3) is that 1:5~20 mix according to volume ratio by the chitosan solution and PLA solution, 10~30min of magnetic agitation freezes 10~12h under the conditions of -10~-18 DEG C, obtains polylactic acid-chitose fiber gel；(4) above-mentioned polylactic acid-chitose fiber gel is carried out to water to replace 6~8 times at 0~4 DEG C, it is subsequently poured into bracket mould, 2~5h is freezed under the conditions of -10~-18 DEG C, finally in 0~5 DEG C of low temperature drying 12~demoulding for 24 hours, washing, obtains polylactic acid-chitose fibrous framework.The porosity for the polylactic acid-chitose fiber scaffold material that method in the present invention is prepared is higher, mechanical property is good, has good biocompatibility.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation of polylactic acid-chitose fiber scaffold material
Method.
Background technique
Material for tissue engineering bracket mainly has natural macromolecular material and synthesis high molecular material, the former generally has
There is preferable cellular affinity, but cause properties of product to be difficult to reappear due to the source of material difference, processing method difference etc.,
The controllable range of its conventional physico-chemical properties is very limited, and opereating specification is relatively narrow in process also limits it in special-shaped material
Application；Synthesis high molecular material has good processing performance and can be by the composition and synthesis process of adjusting product
Technological parameter, and its physicochemical property is enable to regulate and control.But due to such material surface lacks cell recognition site etc., influence
The adherency and growth of cell on the surface thereof.Therefore, biomedical material is modified affine to improve the cell of material
Property, machinability and mechanical property research just become life science and the common research hotspot of material science.And function admirable
The successful exploitation of tissue engineering rack material wound and plastic surgery will be made to enter a brand-new field.
Chitosan is unique a kind of positively charged alkaline polysaccharide present in nature, nontoxic, non-stimulated, is had good
Biocompatibility, biodegradability.Cartilage cell's apposition growth on chitin fiber rack is rapid, and keeps it good
Gene phenotype.Polylactic acid molecule amount is adjustable, and processing performance is excellent, has obtained FDA's as sutures and bone nail etc.
Approve.But its hydrophily difference and catabolite also limit the use of polylactic acid in the disadvantages of acidity.In order to make full use of shell poly-
The excellent mechanical property and machinability of bioactivity and polylactic acid of sugar, people using different methods be made chitosan with
The graft copolymer of polylactic acid.But polylactic acid-chitose brace aperture rate and power that method in the prior art is prepared
It is not ideal enough to learn performance.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of polylactic acid-chitose fiber scaffold material,
It is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of polylactic acid-chitose fiber scaffold material, existing to overcome
There is the deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of polylactic acid-chitose fiber scaffold material, comprising:
(1) it prepares PLA solution: acetone soln is added in polylactic acid, it is molten to obtain polylactic acid by 60~90min of magnetic agitation
Liquid；
(2) it prepares chitosan solution: chitosan is added to the water, stir 10~20min, obtain chitosan solution；
It (3) is that 1:5~20 mix according to volume ratio by the chitosan solution and PLA solution, magnetic agitation 10
~30min freezes 10~12h under the conditions of -10~-18 DEG C, obtains polylactic acid-chitose fiber gel；
(4) above-mentioned polylactic acid-chitose fiber gel is carried out to water to replace 6~8 times at 0~4 DEG C, is subsequently poured into bracket
In mold, 2~5h is freezed under the conditions of -10~-18 DEG C, finally in 0~5 DEG C of low temperature drying 12~demoulding for 24 hours, washing, is obtained
Polylactic acid-chitose fibrous framework.
Preferably, in step (1), the preparation method of the polylactic acid include: 1) using lactic acid as raw material, temperature be 60~
180 DEG C of 1~8h of dehydrated under vacuum is 130~200 DEG C in temperature using stannous acetate and sulfoacid compound as composite catalyst
Vacuum under melt polymerization 3~for 24 hours, obtain precondensation product；2) by precondensation product in the case where temperature is 90~180 DEG C of vacuum
8~120h of solid phase, obtains polylactic acid.
Preferably, in step (1), the concentration of the polylactic acid are as follows: contain 0.1~0.3 gram of polylactic acid in every milliliter of acetone.
Preferably, in step (2), the concentration of the chitosan are as follows: contain 0.1~0.5 gram of chitosan in every milliliter of water.
Preferably, the sulfoacid compound is selected from one of methanesulfonic acid, ethanesulfonic acid or p-methyl benzenesulfonic acid.
Preferably, the lactic acid is the mixture of Pfansteihl, D-ALPHA-Hydroxypropionic acid or Pfansteihl and D-ALPHA-Hydroxypropionic acid.
Compared with the prior art, the advantages of the present invention are as follows: the polylactic acid-chitose that the method in the present invention is prepared
The porosity of fiber scaffold material is higher, mechanical property is good, has good biocompatibility.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of polylactic acid-chitose fiber scaffold material, comprising:
(1) it prepares PLA solution: acetone soln is added in polylactic acid, it is molten to obtain polylactic acid by 60~90min of magnetic agitation
Liquid；
(2) it prepares chitosan solution: chitosan is added to the water, stir 10~20min, obtain chitosan solution；
It (3) is that 1:5~20 mix according to volume ratio by the chitosan solution and PLA solution, magnetic agitation 10
~30min freezes 10~12h under the conditions of -10~-18 DEG C, obtains polylactic acid-chitose fiber gel；
(4) above-mentioned polylactic acid-chitose fiber gel is carried out to water to replace 6~8 times at 0~4 DEG C, is subsequently poured into bracket
In mold, 2~5h is freezed under the conditions of -10~-18 DEG C, finally in 0~5 DEG C of low temperature drying 12~demoulding for 24 hours, washing, is obtained
Polylactic acid-chitose fibrous framework.
In above-mentioned steps (1), the concentration of the polylactic acid are as follows: contain 0.1~0.3 gram of polylactic acid in every milliliter of acetone, it is excellent
Choosing, the concentration of the polylactic acid are as follows: contain 0.25 gram of polylactic acid in every milliliter of acetone.
In above-mentioned steps (2), the concentration of the chitosan are as follows: contain 0.1~0.5 gram of chitosan in every milliliter of water, preferably
, the concentration of the chitosan are as follows: contain 0.5 gram of chitosan in every milliliter of water.
In one embodiment, in step (1), the preparation method of the polylactic acid includes: 1) using lactic acid as raw material, in temperature
For 60~180 DEG C of 1~8h of dehydrated under vacuum, using stannous acetate and sulfoacid compound as composite catalyst, temperature be 130~
Melt polymerization 3 under 200 DEG C of vacuum~for 24 hours, obtain precondensation product；It 2) is 90~180 DEG C in temperature by precondensation product
8~120h of solid phase under vacuum, obtains polylactic acid.
Wherein, the sulfoacid compound is selected from one of methanesulfonic acid, ethanesulfonic acid or p-methyl benzenesulfonic acid, and the lactic acid is L-
The mixture of lactic acid, D-ALPHA-Hydroxypropionic acid or Pfansteihl and D-ALPHA-Hydroxypropionic acid.
Embodiment
1, polylactic acid is prepared
1) using lactic acid as raw material, the dehydrated under vacuum 5h for being 120 DEG C in temperature is with stannous acetate and ethanesulfonic acid compound
Composite catalyst, the melt polymerization 12h in the case where temperature is 160 DEG C of vacuum, obtains precondensation product；
2) by precondensation product in the case where temperature is 130 DEG C of vacuum solid phase 60h, obtain polylactic acid.
2, polylactic acid-chitose fiber scaffold material is prepared
(1) (1) prepares PLA solution: acetone soln is added in polylactic acid, 60~90min of magnetic agitation obtains poly- cream
Acid solution, wherein contain 0.25 gram of polylactic acid in every milliliter of acetone；
(2) it prepares chitosan solution: chitosan is added to the water, stir 10~20min, obtain chitosan solution, wherein
Contain 0.5 gram of chitosan in every milliliter of water；
It (3) is that 1:10 is mixed according to volume ratio by the chitosan solution and PLA solution, magnetic agitation
20min freezes 12h under the conditions of -15 DEG C, obtains polylactic acid-chitose fiber gel；
(4) above-mentioned polylactic acid-chitose fiber gel is carried out to water to replace 8 times at 4 DEG C, is subsequently poured into bracket mould
In, 3h is freezed under the conditions of -15 DEG C, finally in 4 DEG C of low temperature drying 20h demouldings, washings, obtains polylactic acid-chitose fiber branch
Frame.
The polylactic acid-chitose fiber scaffold material that method in the present invention is prepared has nanofiber and micron openings
The structural form that gap coexists, therefore, timbering material porosity with higher compared with；Meanwhile chitin fiber effectively enhances
The compression modulus of timbering material, so that the timbering material has preferably mechanical property.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (6)
1. a kind of preparation method of polylactic acid-chitose fiber scaffold material characterized by comprising
(1) it prepares PLA solution: acetone soln is added in polylactic acid, 60~90min of magnetic agitation obtains PLA solution；
(2) it prepares chitosan solution: chitosan is added to the water, stir 10~20min, obtain chitosan solution；
It (3) is that 1:5~20 mix according to volume ratio by the chitosan solution and PLA solution, magnetic agitation 10~
30min freezes 10~12h under the conditions of -10~-18 DEG C, obtains polylactic acid-chitose fiber gel；
(4) above-mentioned polylactic acid-chitose fiber gel is carried out to water to replace 6~8 times at 0~4 DEG C, is subsequently poured into bracket mould
In, 2~5h is freezed under the conditions of -10~-18 DEG C, finally in 0~5 DEG C of low temperature drying 12~demoulding for 24 hours, washing, obtains poly- cream
Acid-chitin fiber bracket.
2. the preparation method of polylactic acid-chitose fiber scaffold material according to claim 1, which is characterized in that step
(1) in, the preparation method of the polylactic acid includes: the dehydrated under vacuum 1 for being 60~180 DEG C in temperature 1) using lactic acid as raw material
~8h, using stannous acetate and sulfoacid compound as composite catalyst, in the case where temperature is 130~200 DEG C of vacuum melt polymerization 3~
For 24 hours, precondensation product is obtained；2) by precondensation product in the case where temperature is 90~180 DEG C of vacuum 8~120h of solid phase, obtain
To polylactic acid.
3. the preparation method of polylactic acid-chitose fiber scaffold material according to claim 1, which is characterized in that step
(1) in, the concentration of the polylactic acid are as follows: contain 0.1~0.3 gram of polylactic acid in every milliliter of acetone.
4. the preparation method of polylactic acid-chitose fiber scaffold material according to claim 1, which is characterized in that step
(2) in, the concentration of the chitosan are as follows: contain 0.1~0.5 gram of chitosan in every milliliter of water.
5. the preparation method of polylactic acid-chitose fiber scaffold material according to claim 2, which is characterized in that described
Sulfoacid compound is selected from one of methanesulfonic acid, ethanesulfonic acid or p-methyl benzenesulfonic acid.
6. the preparation method of polylactic acid-chitose fiber scaffold material according to claim 2, which is characterized in that described
Lactic acid is the mixture of Pfansteihl, D-ALPHA-Hydroxypropionic acid or Pfansteihl and D-ALPHA-Hydroxypropionic acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710681147.5A CN109381747A (en) | 2017-08-10 | 2017-08-10 | A kind of preparation method of polylactic acid-chitose fiber scaffold material |
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| CN201710681147.5A CN109381747A (en) | 2017-08-10 | 2017-08-10 | A kind of preparation method of polylactic acid-chitose fiber scaffold material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040259972A1 (en) * | 2003-06-20 | 2004-12-23 | Ringeisen Timothy A. | High density fibrous polymers suitable for implant |
| CN101376687A (en) * | 2007-08-30 | 2009-03-04 | 东丽纤维研究所（中国）有限公司 | Method for preparing polylactic acid |
| CN101411900A (en) * | 2008-11-07 | 2009-04-22 | 青岛大学 | Method for preparing nano stent enhanced by chitosan short fibre |
| CN101693124A (en) * | 2009-10-14 | 2010-04-14 | 重庆文理学院 | Preparation method of polylactic acid/chitosan/carbon fiber porous supports |
| CN105536075A (en) * | 2016-02-27 | 2016-05-04 | 青岛大学 | Nano-micron fiber, chitosan and polylactic acid composite stent and making method thereof |
| CN105641744A (en) * | 2016-02-27 | 2016-06-08 | 青岛大学 | Nano-micro multi-scale chitosan and polylactic acid composite scaffold and preparation method thereof |
-
2017
- 2017-08-10 CN CN201710681147.5A patent/CN109381747A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040259972A1 (en) * | 2003-06-20 | 2004-12-23 | Ringeisen Timothy A. | High density fibrous polymers suitable for implant |
| CN101376687A (en) * | 2007-08-30 | 2009-03-04 | 东丽纤维研究所（中国）有限公司 | Method for preparing polylactic acid |
| CN101411900A (en) * | 2008-11-07 | 2009-04-22 | 青岛大学 | Method for preparing nano stent enhanced by chitosan short fibre |
| CN101693124A (en) * | 2009-10-14 | 2010-04-14 | 重庆文理学院 | Preparation method of polylactic acid/chitosan/carbon fiber porous supports |
| CN105536075A (en) * | 2016-02-27 | 2016-05-04 | 青岛大学 | Nano-micron fiber, chitosan and polylactic acid composite stent and making method thereof |
| CN105641744A (en) * | 2016-02-27 | 2016-06-08 | 青岛大学 | Nano-micro multi-scale chitosan and polylactic acid composite scaffold and preparation method thereof |
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