CN104311848A - Preparation method of regenerated fibroin-nano titanium oxide composite membrane - Google Patents
Preparation method of regenerated fibroin-nano titanium oxide composite membrane Download PDFInfo
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- CN104311848A CN104311848A CN201410499620.4A CN201410499620A CN104311848A CN 104311848 A CN104311848 A CN 104311848A CN 201410499620 A CN201410499620 A CN 201410499620A CN 104311848 A CN104311848 A CN 104311848A
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Abstract
The invention discloses a preparation method of a regenerated fibroin-nano titanium oxide composite membrane. The preparation method contains the following steps: carrying out degumming pretreatment on silk by a soap-alkali method; immersing treated silk in an aqueous solution of calcium chloride, and boiling to obtain a silk fibroin coarse solution; putting the silk fibroin coarse solution obtained into a fibroin fiber dialysis membrane to carrying out dialysis for 2-3 days, and removing Ca<2+>, Cl<-> and some insoluble substances so as to obtain a fibroin solution; and adding a tetrabutyl titanate solution and an ethanol solution drop by drop into the above fibroin solution, carrying out ultrasonic agitation for 30 min, uniformly mixing, taking a few amount of a mixed solution by the use of a transfer pipette and adding the mixed solution drop by drop into a 120mm polystyrene culture dish, removing bubbles, leveling to form gel, and moving the culture dish into a thermostatic drier box and drying so as to obtain the regenerated fibroin-nano titanium oxide composite membrane The composite membrane prepared by the above method has good mechanical property, reduced water-dissolved rate and good biocompatibility. In addition, the preparation method is simple and low-cost.
Description
Technical field:
The present invention relates to pharmaceutical film preparation field, relate to the preparation method of a kind of regenerated silk-nano oxidized titanium compound film specifically.
Background technology:
Silk has good biocompatibility, mechanical property and certain biological degradability, therefore has a wide range of applications at bioengineering field, such as, be widely used in the aspects such as enzyme immobilization, artificial skin, prosthetic ligament and organizational project.But the regenerated silk film that fibroin obtains after dissolving is resistance to water-soluble poor with mechanical property, makes it apply and is restricted.Traditional method is that fibroin and other materials are prepared into matrix material, and as chitosan etc., but fibroin and other macromolecular material compounds can have influence on the biocompatibility of film.
Nano composite material has the character that the normal matrix material such as unique dimensional effect, local fields effect and quantum effect does not possess.Research shows, the reinforce of nano-scale can improve the performance of matrix material in wide region, and nano-titanium oxide is the inorganic nano material that research is the most active at present, has the advantage such as long acting antibiotic, shielding ultraviolet rays,, general for the field such as makeup, antibacterial fiber.Therefore, in Fibroin Films, add nano-titanium oxide, improve mechanical property and the water tolerance of regenerated silk film.
Summary of the invention:
For solving the problem, the invention provides the preparation method of a kind of regenerated silk-nano oxidized titanium compound film.Composite membrane good mechanical property prepared by the method, water dissolve-loss ratio reduces, good biocompatibility, and preparation method is simple, and cost is low.
Object of the present invention is achieved through the following technical solutions:
A preparation method for regenerated silk-nano oxidized titanium compound film, is characterized in that comprising the following steps:
(1) soap-alkaline process is utilized by silk to carry out coming unstuck pre-treatment;
(2) Silk Soaking after process, in calcium chloride water, boils and boils, obtain the thick lysate of fibroin;
(3) the thick lysate of fibroin obtained is loaded in fibroin fiber dialysis membrane, dialysis 2-3 days, removing Ca
2+, Cl
-with some insolubless, obtain fibroin lysate;
(4) in above-mentioned fibroin lysate, tetrabutyl titanate solution and ethanolic soln is dripped, ultrasonic agitation 30min mixes, be added drop-wise in 120mm polystyrene culture dish with the transfer pipet mixing solutions that takes a morsel, remove bubble, after smooth formation gel, move in thermostatic drying chamber, dry, obtain regenerated silk-nano oxidized titanium compound film.
Preferred as technique scheme, in step (2), the mass concentration of calcium chloride is 10 ~ 30%.
Preferred as technique scheme, in step (2), boiling temperature is 60 ~ 70 DEG C, and the time of boiling of boiling is 2 ~ 3h.
Preferred as technique scheme, in step (3), dialysis time is 3 days.
Preferred as technique scheme, in step (4), the volume ratio of tetrabutyl titanate and ethanol is 1:5.
Preferred as technique scheme, the container preparing composite membrane in step (4) is polystyrene culture dish.
Preferred as technique scheme, the nano-titanium oxide particle diameter that step (5) generates is within 10nm.
Beneficial effect of the present invention is: in fibroin lysate, add machine nano-titanium oxide, improves the degree of crystallinity of fibroin, thus improves the resistance to water-soluble of fibroin and its mechanical property.The method preparation is simple, and cost is low, the good biocompatibility of the composite membrane of preparation, and has certain biological degradability.
Embodiment:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only for explaining the present invention, does not form limiting the scope of the present invention.
Embodiment 1
(1) soap-alkaline process is utilized by silk to carry out coming unstuck pre-treatment;
(2) Silk Soaking after process is in the calcium chloride water of 10% in concentration, and 60 DEG C boil and boil 2h, obtain the thick lysate of fibroin;
(3) the thick lysate of fibroin obtained is loaded in fibroin fiber dialysis membrane, dialyse 2 days, removing Ca
2+, Cl
-with some insolubless, obtain fibroin lysate;
(4) in above-mentioned fibroin lysate, 1mL tetrabutyl titanate solution is dripped, 5mL ethanolic soln, ultrasonic agitation 30min mixes, be added drop-wise in 120mm polystyrene culture dish with the transfer pipet mixing solutions that takes a morsel, remove bubble, after smooth formation gel, move in thermostatic drying chamber, 80 DEG C of oven dry, obtain regenerated silk-nano oxidized titanium compound film.
Embodiment 2
(1) soap-alkaline process is utilized by silk to carry out coming unstuck pre-treatment;
(2) Silk Soaking after process is in the calcium chloride water of 30% in concentration, and 70 DEG C boil and boil 3h, obtain the thick lysate of fibroin;
(3) the thick lysate of fibroin obtained is loaded in fibroin fiber dialysis membrane, dialyse 3 days, removing Ca
2+, Cl
-with some insolubless, obtain fibroin lysate;
(4) in above-mentioned fibroin lysate, 2mL tetrabutyl titanate solution is dripped, 10mL ethanolic soln, ultrasonic agitation 30min mixes, be added drop-wise in 120mm polystyrene culture dish with the transfer pipet mixing solutions that takes a morsel, remove bubble, after smooth formation gel, move in thermostatic drying chamber, 80 DEG C of oven dry, obtain regenerated silk-nano oxidized titanium compound film.
Embodiment 3
(1) soap-alkaline process is utilized by silk to carry out coming unstuck pre-treatment;
(2) Silk Soaking after process is in the calcium chloride water of 20% in concentration, and 65 DEG C boil and boil 2.5h, obtain the thick lysate of fibroin;
(3) the thick lysate of fibroin obtained is loaded in fibroin fiber dialysis membrane, dialyse 2 days, removing Ca
2+, Cl
-with some insolubless, obtain fibroin lysate;
(4) in above-mentioned fibroin lysate, 3mL tetrabutyl titanate solution is dripped, 15mL ethanolic soln, ultrasonic agitation 30min mixes, be added drop-wise in 120mm polystyrene culture dish with the transfer pipet mixing solutions that takes a morsel, remove bubble, after smooth formation gel, move in thermostatic drying chamber, 80 DEG C of oven dry, obtain regenerated silk-nano oxidized titanium compound film.
Claims (7)
1. a preparation method for regenerated silk-nano oxidized titanium compound film, is characterized in that comprising the following steps:
(1) soap-alkaline process is utilized by silk to carry out coming unstuck pre-treatment;
(2) Silk Soaking after process, in calcium chloride water, boils and boils, obtain the thick lysate of fibroin;
(3) the thick lysate of fibroin obtained is loaded in fibroin fiber dialysis membrane, dialysis 2-3 days, removing Ca
2+, Cl
-with some insolubless, obtain fibroin lysate;
(4) in above-mentioned fibroin lysate, tetrabutyl titanate solution and ethanolic soln is dripped, ultrasonic agitation 30min mixes, be added drop-wise in 120mm polystyrene culture dish with the transfer pipet mixing solutions that takes a morsel, remove bubble, after smooth formation gel, move in thermostatic drying chamber, dry, obtain regenerated silk-nano oxidized titanium compound film.
2. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: in step (2), the mass concentration of calcium chloride is 10 ~ 30%.
3. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: in step (2), boiling temperature is 60 ~ 70 DEG C, and the time of boiling of boiling is 2 ~ 3h.
4. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: in step (3), dialysis time is 3 days.
5. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: in step (4), the volume ratio of tetrabutyl titanate and ethanol is 1:5.
6. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: the container preparing composite membrane in step (4) is polystyrene culture dish.
7. the preparation method of a kind of regenerated silk as claimed in claim 1-nano oxidized titanium compound film, is characterized in that: the nano-titanium oxide particle diameter that step (5) generates is within 10nm.
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| CN201410499620.4A CN104311848A (en) | 2014-09-25 | 2014-09-25 | Preparation method of regenerated fibroin-nano titanium oxide composite membrane |
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Cited By (5)
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| CN104611913A (en) * | 2015-02-03 | 2015-05-13 | 湖州新创丝织品有限公司 | Preparation method of novel multifunctional silk filtering material |
| CN105544209A (en) * | 2016-01-21 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Textile after-finishing process taking silk fibroin as medium |
| CN106592012A (en) * | 2016-12-06 | 2017-04-26 | 宁波芸生纺织品科技有限公司 | Biological fiber material and preparation method thereof |
| CN106732808A (en) * | 2016-11-25 | 2017-05-31 | 江苏爱西施科技服务咨询股份有限公司 | A kind of fibroin albumen/TiO2The preparation method of composite catalyst |
| WO2019066037A1 (en) * | 2017-09-29 | 2019-04-04 | Ｓｐｉｂｅｒ株式会社 | Dope liquid and product using same, and structural protein fiber and method for producing same |
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| CN102702727A (en) * | 2012-06-26 | 2012-10-03 | 重庆理工大学 | Preparation method for antibacterial composite material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104611913A (en) * | 2015-02-03 | 2015-05-13 | 湖州新创丝织品有限公司 | Preparation method of novel multifunctional silk filtering material |
| CN104611913B (en) * | 2015-02-03 | 2016-09-07 | 重庆绿草缘皮革制品有限公司 | A kind of preparation method of Multifunctional silk filtering material |
| CN105544209A (en) * | 2016-01-21 | 2016-05-04 | 苏州印丝特纺织数码科技有限公司 | Textile after-finishing process taking silk fibroin as medium |
| CN106732808A (en) * | 2016-11-25 | 2017-05-31 | 江苏爱西施科技服务咨询股份有限公司 | A kind of fibroin albumen/TiO2The preparation method of composite catalyst |
| CN106592012A (en) * | 2016-12-06 | 2017-04-26 | 宁波芸生纺织品科技有限公司 | Biological fiber material and preparation method thereof |
| CN109468705A (en) * | 2016-12-06 | 2019-03-15 | 宁波芸生纺织品科技有限公司 | A kind of biological fibrous material |
| CN109468705B (en) * | 2016-12-06 | 2020-12-29 | 宁波芸生纺织品科技有限公司 | Biological fiber material |
| WO2019066037A1 (en) * | 2017-09-29 | 2019-04-04 | Ｓｐｉｂｅｒ株式会社 | Dope liquid and product using same, and structural protein fiber and method for producing same |
| JPWO2019066037A1 (en) * | 2017-09-29 | 2020-11-05 | Ｓｐｉｂｅｒ株式会社 | Doping solution, products using it, structural protein fiber and its manufacturing method |
| JP7231939B2 (en) | 2017-09-29 | 2023-03-02 | Ｓｐｉｂｅｒ株式会社 | Dope solution and product using the same, structural protein fiber and method for producing the same |
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Application publication date: 20150128 |