CN108786491A - A kind of poly-dopamine/triclosan/titania coextruded film and preparation method thereof - Google Patents
A kind of poly-dopamine/triclosan/titania coextruded film and preparation method thereof Download PDFInfo
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- CN108786491A CN108786491A CN201810558397.4A CN201810558397A CN108786491A CN 108786491 A CN108786491 A CN 108786491A CN 201810558397 A CN201810558397 A CN 201810558397A CN 108786491 A CN108786491 A CN 108786491A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/60—Polyamines
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2325/48—Antimicrobial properties
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Abstract
The invention discloses a kind of poly-dopamine/triclosan/titania coextruded films and preparation method thereof, belong to material surface modifying technology field.The preparation method is that based on mixed solvent method and co-electrodeposition method in situ, including preparing dopamine-Tris buffer solutions, triclosan-ethanol solution and TiO 2 precursor colloidal sol, first dopamine-Tris buffer solutions are mixed with triclosan-ethanol solution, add TiO 2 precursor colloidal sol, mixed solution is formed, then substrate is put into taking-up drying after being impregnated in mixed solution can be obtained poly-dopamine/triclosan/titania coextruded film.The method for manufacturing thin film of the present invention is simple, it is mild to prepare environment, obtained film has good hydrophily, excellent biocompatibility, and certain anti-microbial property is had both, it has some improvement to substrate surface, can be applied to the biomedical engineering fields such as Cell culture invitro, organizational project.
Description
Technical field
The invention belongs to bio-medical film applications, and in particular to a kind of poly-dopamine/triclosan/titanium dioxide THIN COMPOSITE
Film and preparation method thereof, the film have both excellent biocompatibility and antibiotic property.
Background technology
DOPA amine monomers are derived from a kind of adhesive function unit in mussel adhesion protein, can autohemagglutination film forming, have it is good
Good adhesiveness, and containing in poly-dopamine (PDA) structure largely can be as the phenolic hydroxyl group and amine of second order reaction platform
Base group, thus can greatly improve adhesion material surface hydrophily and biocompatibility [Crisp D J, Walker G,
Young G A,et al.Adhesion and substrate choice in mussels and barnacles[J]
.Journal of Colloid&Interface Science,1985,104(1):40-50.]；Titanium dioxide is a kind of nontoxic
, material with good biocompatibility and chemical stability, be widely used and have developed rapidly in the field of medicine.
Cell culture experiments the result shows that, TiO2Coating has good biocompatibility [Dieudonne S C, Van den
Dolder J,De Ruijter J E et al.Biomaterials[J],2002,23(14):3041], no cytotoxicity.
In the practical application of bio-medical material, it usually will appear inflammatory reaction and bacterium sense after material implantation human body
Dye, therefore, the antibiotic property of material surface is increasingly becoming research hotspot.Triclosan as a kind of external application high-efficiency antimicrobial disinfectant, it
The fungies such as the bacteriums such as staphylococcus aureus, Escherichia coli and Candida albicans can be killed, in addition, triclosan to virus (such as
Hepatitis type B virus etc.) also there is supression effect.
The solubility of triclosan in water is extremely low (≈ 4.62mg/L), and itself can not be adhered to material surface, binding force
Very poor, how triclosan is combined to material surface becomes key.
Invention content
Have excellent hydrophilic, preparation method simple the object of the present invention is to provide one kind and has both excellent bio-compatible
Poly-dopamine/triclosan/titania coextruded film and preparation method thereof of property and antibiotic property, this method can be applied to material table
Face is modified, at low cost.
Heretofore described poly-dopamine/triclosan/titania coextruded film, be by poly-dopamine, triclosan and
Titanium dioxide is made using mixed solvent method in substrate.
The substrate is either rigid basement, such as quartz glass, or flexible substrates, such as PS substrates, especially
The extremely low base materials of surface energies such as polytetrafluoroethylene (PTFE) can also be applied to by being this method.
The method for preparing the poly-dopamine/triclosan/titania coextruded film, steps are as follows：
1) first Tris and dopamine are sequentially added and forms buffer solution in deionized water, a concentration of 8~12mM of Tris is more
A concentration of 1~3g/L of bar amine, the pH for adjusting solution are 8.5；Compound concentration is that triclosan-ethanol solution of 1~3g/L is for use；
2) dopamine-Tris buffer solutions and triclosan-ethanol solution are mixed, magneton is used in combination to stir evenly, add 8~
12mL TiO 2 sols continue magnetic agitation and form mixed solution；
3) substrate after cleaning is immersed in mixed solution after 22~26h, takes out substrate, it is dry, obtain poly-dopamine/tri-
Chlorine life/titania coextruded film.
The volume ratio of the dopamine-Tris buffer solutions and triclosan-ethanol solution that are added is 35:2~35:10, it is made
Laminated film with excellent biocompatibility and anti-microbial property, when triclosan content is relatively low in entire thin film system,
The antibiotic property of film is difficult to reach requirement, and when its content higher, though there is preferable anti-microbial property, its biocompatibility
It is poor.
Heretofore described TiO 2 sol is that titania nanoparticles are scattered in deionized water, a concentration of
0.5mol/L~1mol/L.
The present invention uses mixed solvent method, and dopamine-Tris buffer solutions and triclosan-ethanol solution are mixed to form mixing
Solution, and TiO 2 sol is added, using the intersolubility of water and ethyl alcohol, dopamine utilizes poly-dopamine in the course of the polymerization process
Triclosan and titanium dioxide are bonded in material surface by auto polymerization filming performance and adhesiveness, obtain being firmly combined with substrate and simultaneous
Have excellent biocompatibility and poly-dopamine/triclosan/titania coextruded film of antibiotic property.Present invention incorporates poly- DOPA
The adhesiveness of amine, the high-efficiency antimicrobial of triclosan and the good biocompatibility of titanium dioxide, hydrophily, improve substrate surface
Hydrophily, cell compatibility and anti-microbial property, cell material surface adsorb it is all right.Method of the present invention
At low cost for mixed solvent method and co-electrodeposition method in situ, it is mild to prepare environment, easy to operate, has certain modified make to substrate
With the biomedical engineering fields such as Cell culture invitro, organizational project can be preferably applied for.
Description of the drawings
Fig. 1 is the SEM figures after obtaining poly-dopamine/titania coextruded film in embodiment 1 on ptfe substrate.
Fig. 2 is after obtaining poly-dopamine/triclosan/titania coextruded film in embodiment 2 on ptfe substrate
SEM figure.
Fig. 3 is ptfe substrate and poly-dopamine/titanium deoxid film and poly-dopamine/tri- made from its surface
Hydrophily variation diagram of the chlorine life/titania coextruded film before and after ultraviolet irradiation.
Fig. 4 is on ptfe substrate and poly-dopamine/triclosan/titania coextruded film made from its surface
Cultivate the OD values after fibroblast 1d, 3d.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention will be described in detail, but the present invention is not limited to this.
Embodiment 1
1) first using deionized water as solvent, a certain amount of Tris, concentration 8mM are first added into 200ml deionized waters, adjusts
It is 8.5 to save pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) it takes 10ml to be added thereto after TiO 2 sol being diluted to 0.5mol/L with deionized water, is stirred with magneton mixed
It closes uniform；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/titania coextruded film.Its SEM figure is shown in Fig. 1.
Embodiment 2
1) first using deionized water as solvent, a certain amount of Tris, concentration 8mM are first added into 200ml deionized waters, adjusts
It is 8.5 to save pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.2g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 2g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:2 ratio is uniformly mixed, and makes total volume
For 100ml, takes 10ml to be added thereto after TiO 2 sol is then diluted to 0.5mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.Its SEM figure is shown in Fig. 2.
This example is compared with embodiment 1, from the basic phase of surface topography of laminated film after visible addition triclosan in SEM figures
Together, titania nanoparticles are evenly distributed, and will not change its pattern substantially using film made from the method for the present invention, be conducive to
Its subsequent applications.
Embodiment 3
1) first using deionized water as solvent, a certain amount of Tris, concentration 8mM are first added into 200ml deionized waters, adjusts
It is 8.5 to save pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.2g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 2g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:6 ratio is uniformly mixed, and makes total volume
For 100ml, takes 10ml to be added thereto after TiO 2 sol is then diluted to 0.5mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Hydrophily test is carried out respectively before and after ultraviolet irradiation to sample made from this example, and result and example 1, example 2 are made
The sample obtained carries out hydrophily test acquired results before and after ultraviolet irradiation and compares, and water contact angle variation diagram (such as Fig. 3) is made.
As seen from the figure, after thin film being made on ptfe substrate hydrophily has a degree of improvement, and gained is answered
Closing has the presence of titanium dioxide in film.
Embodiment 4
1) first using deionized water as solvent, a certain amount of Tris, concentration 10mM are first added into 200ml deionized waters,
It is 8.5 to adjust pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.2g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 2g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:6 ratio is uniformly mixed, and makes total volume
For 100ml, takes 10ml to be added thereto after TiO 2 sol is then diluted to 0.5mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed for 24 hours, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Respectively the film made from this example, film obtained in embodiment 8, carry out into fiber on ptfe substrate
Cell injuring model after cultivating 1d, 3d, utilizes CCK-8 (Cell Counting Kit-8) method to measure OD values (Optical
Density, also known as light absorption value), the OD values of film made from this example have obvious increasing compared to the OD values of ptfe substrate
Add and illustrate that the biocompatibility of obtained laminated film improves compared to substrate (see Fig. 4), has to substrate certain
Modifying function.The OD values of the film of gained are declined instead compared to ptfe substrate in embodiment 8, illustrate to work as triclosan
When too high levels, though having preferable anti-microbial property, its biocompatibility is poor.
Embodiment 5
1) first using deionized water as solvent, a certain amount of Tris, concentration 10mM are first added into 200ml deionized waters,
It is 8.5 to adjust pH value of solution, then is charged with 0.2g dopamines, makes a concentration of 1g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.2g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 2g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:8 ratio is uniformly mixed, and makes total volume
For 100ml, takes 10ml to be added thereto after TiO 2 sol is then diluted to 0.8mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed for 24 hours, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Embodiment 6
1) first using deionized water as solvent, a certain amount of Tris, concentration 12mM are first added into 200ml deionized waters,
It is 8.5 to adjust pH value of solution, then is charged with 0.6g dopamines, makes a concentration of 3g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.3g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 3g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:10 ratio is uniformly mixed, and makes total volume
For 100ml, takes 8ml to be added thereto after TiO 2 sol is then diluted to 1.0mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed 26h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Embodiment 7
1) first using deionized water as solvent, a certain amount of Tris, concentration 12mM are first added into 200ml deionized waters,
It is 8.5 to adjust pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.1g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 1g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:10 ratio is uniformly mixed, and makes total volume
For 100ml, takes 12ml to be added thereto after TiO 2 sol is then diluted to 0.8mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Embodiment 8
1) first using deionized water as solvent, a certain amount of Tris, concentration 12mM are first added into 200ml deionized waters,
It is 8.5 to adjust pH value of solution, then is charged with 0.4g dopamines, makes a concentration of 2g/L of dopamine in solution, obtains dopamine-
Tris buffer solutions；
2) 0.1g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 1g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris buffer solutions and triclosan-ethanol solution:12 ratio is uniformly mixed, and makes total volume
For 100ml, takes 12ml to be added thereto after TiO 2 sol is then diluted to 0.8mol/L with deionized water, stirred with magneton
It is uniformly mixed；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h obtains poly-dopamine/triclosan/titania coextruded film.
Embodiment 9
1) first using absolute ethyl alcohol as solvent, a certain amount of Tris, concentration 12mM are first added into 200ml ethyl alcohol, adjusts
PH value of solution is 8.5, then is charged with 0.4g dopamines, obtains dopamine-Tris buffer solutions；
2) 0.1g triclosans are added into 100ml absolute ethyl alcohols, makes a concentration of 1g/L of triclosan in solution, takes respectively more
The two is 35 by volume by bar amine-Tris ethanol solutions and triclosan-ethanol solution:12 ratio is uniformly mixed, and makes totality
Product is 100ml, takes 12ml to be added thereto after TiO 2 sol is then diluted to 0.8mol/L with deionized water, is stirred with magneton
It mixes uniformly mixed；
3) ptfe substrate after cleaning is immersed 22h, then takes out, places it in 60 DEG C of baking ovens and keep the temperature
1h。
In this example, be used only ethanol as solvent when, find dopamine can not autohemagglutination film forming, substrate is immersed immersion
It is unable to get required poly-dopamine/triclosan/titania coextruded film afterwards.And individually use water as solvent then due to three
The solubility of chlorine life in water is extremely low, can not be adhered to material surface, binding force is very poor.The present invention uses mixed solvent method, will
Dopamine-Tris buffer solutions and triclosan-ethanol solution are mixed to form mixed solution, and TiO 2 sol is added, and utilize water
It is with the intersolubility of ethyl alcohol, triclosan is evenly dispersed, by the auto polymerization filming performance of poly-dopamine and adhesiveness by triclosan
It is bonded in material surface with titanium dioxide, obtains being firmly combined with and have both with substrate the poly- more of excellent biocompatibility and antibiotic property
Bar amine/triclosan/titania coextruded film.
Claims (5)
1. a kind of poly-dopamine/triclosan/titania coextruded film, characterized in that by poly-dopamine, triclosan and titanium dioxide
Titanium is made using mixed solvent method in substrate.
2. poly-dopamine/triclosan/titania coextruded film according to claim 1, it is characterised in that the base
Bottom is polytetrafluoroethylene (PTFE), PS substrates, quartz glass.
3. the method for preparing poly-dopamine/triclosan/titania coextruded film described in claim 1, it is characterised in that step
It is rapid as follows：
1) first Tris and dopamine are sequentially added and forms buffer solution in deionized water, a concentration of 8~12mM of Tris, dopamine
A concentration of 1~3g/L, adjust solution pH be 8.5；Compound concentration is that triclosan-ethanol solution of 1~3g/L is for use；
2) dopamine-Tris buffer solutions and triclosan-ethanol solution are mixed, is used in combination magneton to stir evenly, adds 8~12mL
TiO 2 sol continues magnetic agitation and forms mixed solution；
3) substrate after cleaning is immersed in mixed solution after 22~26h, takes out substrate, it is dry, obtain poly-dopamine/trichlorine
Life/titania coextruded film.
4. the preparation method of poly-dopamine/triclosan/titania coextruded film according to claim 3, feature exist
In the dopamine-Tris buffer solutions and triclosan-ethanol solution that are added volume ratio be 35:2~35:10.
5. the preparation method of poly-dopamine/triclosan/titania coextruded film according to claim 3, feature exist
In a concentration of 0.5~1mol/L for the TiO 2 sol being added.
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| CN112225894A (en) * | 2020-10-12 | 2021-01-15 | 江南大学 | Hybrid nano particle, preparation method and anti-ultraviolet application |
| CN112900072A (en) * | 2021-01-25 | 2021-06-04 | 西南大学 | PBO fiber based on bionic modification of ternary codeposition system and preparation method and application thereof |
| CN113698717A (en) * | 2021-09-08 | 2021-11-26 | 江苏景鹊医疗科技有限公司 | Medical polymer material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110280313A (en) * | 2019-07-11 | 2019-09-27 | 哈尔滨工业大学 | A kind of three-dimensional structure load TiO2-xThe preparation method of material |
| CN112225894A (en) * | 2020-10-12 | 2021-01-15 | 江南大学 | Hybrid nano particle, preparation method and anti-ultraviolet application |
| CN112225894B (en) * | 2020-10-12 | 2021-10-15 | 江南大学 | Hybrid nano particle, preparation method and anti-ultraviolet application |
| CN112900072A (en) * | 2021-01-25 | 2021-06-04 | 西南大学 | PBO fiber based on bionic modification of ternary codeposition system and preparation method and application thereof |
| CN113698717A (en) * | 2021-09-08 | 2021-11-26 | 江苏景鹊医疗科技有限公司 | Medical polymer material and preparation method and application thereof |
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| CN108786491B (en) | 2020-09-04 |
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