CN106758217A - A kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane - Google Patents

A kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane Download PDF

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CN106758217A
CN106758217A CN201611270384.4A CN201611270384A CN106758217A CN 106758217 A CN106758217 A CN 106758217A CN 201611270384 A CN201611270384 A CN 201611270384A CN 106758217 A CN106758217 A CN 106758217A
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gelatin
composite nano
fiber membrane
chitosan composite
crosslinking
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蔡宁
韩超
喻发全
付晶
罗晓刚
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Wuhan Institute of Technology
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Wuhan Institute of Technology
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144Alcohols; Metal alcoholates
    • D06M13/148Polyalcohols, e.g. glycerol or glucose
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • D06M15/05Cellulose or derivatives thereof
    • D06M15/09Cellulose ethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres

Abstract

The present invention relates to a kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane, following steps are included:1) preparation of the biological polyoses of oxidation;2) preparation of gelatin/chitosan composite nano-fiber membrane;3) preparation of the gelatin/chitosan composite nano-fiber membrane of crosslinking:By step 1) in the biological polyoses of oxidation that prepare be dissolved in absolute ethyl alcohol, take step 2) in the gelatin/chitosan composite nano-fiber membrane for preparing, it is cut into small pieces and is soaked in the crosslinking medium of the biological polyoses of above-mentioned oxidation, it is crosslinked 1~5 day under the conditions of 0~50 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.Gelatin/chitosan composite nano-fiber membrane obtained in the technique has the characteristic of two components concurrently, and with good mechanical characteristic and water resistance, fibrous body structure is not destroyed after gelatin/chitosan composite nano-fiber membrane soaks through long-time solution.

Description

A kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane
Technical field
The invention belongs to technical field of polymer materials.Specifically related to a kind of gelatin/chitosan composite nano-fiber membrane Crosslinking preparation method.
Background technology
The features such as Electrospun nano-fibers have specific surface area and porosity high, is conducive to absorbing wound exudate, Its less space can prevent the intrusion of bacterium.The 3-D solid structure of nano fibrous membrane can the outer interstitial of analog cell, from And sticking, breed, breaking up for cell can be promoted.Therefore it can be applied to the fields such as wound dressing, organizational project, with good Potential applicability in clinical practice.Gelatin is the class protein as obtained from collagen hydrolysate, has homology with collagen.But It is that compared with collagen, its price is less expensive, and no antigen.Additionally, gelatin has good biocompatibility and biology Degradability, and it can be effectively promoted cell adhesion, propagation and differentiation.Shitosan is the deacetylation derivative of chitin, With excellent biocompatibility and biodegradability, while there is antibacterial anti hemorrhagic, promoting wound healing and cell growth etc. Excellent biological property.In actual application, it usually needs target material has multifrequency nature.In the preparation of nano material During, the characteristic for having each component using two or more component blendings is introduced into composite, so as to assign Prepared composite multifrequency nature, and compensate for mutual defect.By gelatin and compound the receiving of chitosan blend preparation Rice tunica fibrosa not only has the respective advantage of two components concurrently, and it is multiple by electrostatic interaction can to form polyelectrolyte therebetween Compound, improves the mechanical property of intermingling material.
Although gelatin/chitosan composite nano-fiber membrane has many superior performances, due to the hole of nano fibrous membrane The gap rate stronger hydrophily with both higher so that the mechanical property and water resistance of gelatin/chitosan composite nano-fiber membrane Can be not enough, therefore significantly limit its application in field of tissue engineering technology.In the patent of Publication No. CN104894856A just A kind of method of the mechanical property and water resistance of the method lifting nano fibrous membrane using chemical crosslinking is disclosed, although the method The mechanical property of nano fibrous membrane can to a certain extent be strengthened, but be the use of poisonous and hazardous chemical reagent, and existed The problems such as chemical agent residue, generation side reaction.For example, such as granted patent number is CN102558589B and CN102585265B Patent in propose respectively with the method for formaldehyde and glutaraldehyde solution cross-linked gelatin composite membrane, although the method can play compared with The effect of enhancing mechanical property and water resistance well, but the poisonous materials such as formaldehyde and glutaraldehyde are introduced so as to influence it to enter one Walk the application in bio-medical field.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of gelatin/chitosan composite nano-fiber membrane of environmental protection Crosslinking preparation method, its mechanical property and water resistance be improved significantly.
The present invention solves the technical scheme that is used of above-mentioned technical problem:A kind of gelatin/chitosan composite nano fiber The crosslinking preparation method of film, includes following steps:
1) preparation of the biological polyoses of oxidation:
Weigh 0.1~10g strong oxidizers to be dissolved in the aqueous solution of 1~20wt% biological polyoses, under conditions of lucifuge Reaction is stirred vigorously, reacted solution is dialysed 1~5 day, the biology aoxidized after the solution after dialysis is freeze-dried Polysaccharide;
2) preparation of gelatin/chitosan composite nano-fiber membrane:
Gelatin and shitosan are dissolved in acetum respectively, magnetic agitation, respectively obtain concentration for 5~30wt% is equal One transparent gelatin and chitosan solution, is then 1 with mass ratio:9~9:1 ratio obtains two kinds of solution blendings, stirring The electrostatic spinning precursor liquid of transparent and homogeneous, gelatin/shell is prepared by above-mentioned electrostatic spinning precursor liquid by method of electrostatic spinning again Chitosan composite nanometer fibre film;
3) preparation of the gelatin/chitosan composite nano-fiber membrane of crosslinking:
By step 1) in the biological polyoses of oxidation that prepare be dissolved in absolute ethyl alcohol, take step 2) in prepare Gelatin/chitosan composite nano-fiber membrane, be cut into small pieces and be soaked in the crosslinking medium of the biological polyoses of above-mentioned oxidation, It is crosslinked 1~5 day under the conditions of 0~50 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
By such scheme, step 1) described in strong oxidizer be potassium permanganate, sodium metaperiodate, potassium bichromate, potassium chlorate, three Any one in iron chloride or mixture.
By such scheme, step 1) described in biological polyoses be glucan, konjaku glucomannan, carboxymethylcellulose calcium, Portugal Any one in grape sugar or mixture.
By such scheme, step 1) described in reaction condition be 10~50 DEG C, the reaction time be 0.5~24h.
By such scheme, step 2) described in method of electrostatic spinning parameter it is as follows:Temperature be 10~60 DEG C, humidity be 20~ 80%, fltting speed is 0.1~3.0mL/h, and voltage is 10~50kV, and the distance of spinning head to receiver board is 5~30cm.
Traditional cross-linked gelatin/chitosan composite nano fibre film often use poisonous and hazardous chemical aldehyde (such as formaldehyde, Glutaraldehyde) used as crosslinking agent, the biological polyoses of the oxidation used in the inventive method are a kind of environmental protection, nontoxic friendship Connection agent, and without any bio-toxicity.By the present invention in that with oxidation this environmental protection of biological polyoses, nontoxic friendship Connection agent, and the cross-linking method without any bio-toxicity come solve gelatin/chitosan composite nano-fiber membrane fragility greatly, water resistance The problems such as difference, substitute poisonous and harmful conventional at present, the chemical cross-linking agent (such as glutaraldehyde, formaldehyde) with bio-toxicity.Through After the inventive method crosslinking Treatment, the mechanical property and water resistance of gelatin/chitosan composite nano-fiber membrane are substantially changed It is kind.
The present invention is used for cross-linked gelatin/chitosan composite nano fibre using the biological polyoses of the oxidation of no biotoxicity Film, the amino on amino and chitosan molecule chain on aldehyde radical and gelatin chains on the biological polyoses of oxidation is by forming seat Husband's alkali plays a part of crosslinking, so as to reach the mechanical property and water resistance of enhancing gelatin/chitosan composite nano-fiber membrane Energy.Gelatin/chitosan composite nano-fiber membrane obtained in the technique has the characteristic of two components concurrently, and with good mechanical characteristic And water resistance, fibrous body structure is not destroyed after gelatin/chitosan composite nano-fiber membrane soaks through long-time solution. Therefore actual answering can be obtained in bio-medical material through the gelatin/chitosan composite nano-fiber membrane of the inventive method crosslinking Treatment With;The method of the present invention has simple to operate, effect is significant, with low cost, the characteristics of environmental protection, is expected to be used for industrial metaplasia Produce, for quickly and efficiently enhancing composite nano-fiber membrane mechanical property provides a kind of new method.
Brief description of the drawings
Fig. 1 is the scanning electricity before and after the oxidized glucan crosslinking of gelatin/chitosan composite nano-fiber membrane in embodiment 1 Sub- microscope (SEM) figure;
Fig. 2 is the load-deformation curve before and after the oxidized glucose crosslinking of gelatin/chitosan composite nano-fiber membrane;
Fig. 3 is the oxidized carboxymethyl cellulose crosslinked front and rear swelling behavior of gelatin/chitosan composite nano-fiber membrane Figure;
Fig. 4 is the mass loss before and after the oxidized konjaku glucomannan crosslinking of gelatin/chitosan composite nano-fiber membrane Figure.
Specific embodiment
With reference to specific embodiment, the inventive method is expanded on further.It should be understood that these embodiments are merely to illustrate this Invention rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, this area skill Art personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims institute The scope of restriction.
Embodiment 1
(1) weigh 0.1g potassium permanganate to be dissolved in the glucan aqueous solution that mass fraction is 1wt%, in the condition of lucifuge Under be stirred vigorously under the conditions of 10 DEG C reaction 0.5h, by reacted solution dialyse 3 days, the solution after dialysis is freeze-dried The glucan for being aoxidized;
(2) gelatin and shitosan are dissolved separately in the acetum of 90wt%, magnetic agitation, prepare quality point Number is the gelatin and chitosan solution of the transparent and homogeneous of 5wt% and 30wt%;
(3) by the gelatin and chitosan solution described in above-mentioned steps (2) with mass ratio be 1:9 ratio blending, stirs 2h Obtain the electrostatic spinning precursor liquid of transparent and homogeneous;
(4) the above-mentioned solution for preparing is fitted into syringe, and is fixed on the propeller of electrostatic spinning apparatus, passed through Electrostatic spinning prepares gelatin/chitosan composite nano-fiber membrane;The condition of wherein electrostatic spinning is as follows:Spinning temperature is 20 DEG C, Humidity is 20%, and fltting speed is 1.0mL/h, and voltage is 35kV, and the distance of spinning head to receiver board is 10cm;
(5) glucan by the oxidation prepared in step (1) is dissolved in absolute ethyl alcohol, takes a certain amount of step (4) the gelatin/chitosan composite nano-fiber membrane prepared in, the glucan for being cut into rectangle and being soaked in oxidation is handed over In connection medium, it is crosslinked 3 days under the conditions of 37 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
Fig. 1 is that the oxidized glucan crosslinking of gelatin/chitosan composite nano-fiber membrane obtained in embodiment 1 is front and rear to be swept Electron microscope (SEM) figure is retouched, wherein left figure is the SEM figures of uncrosslinked gelatin/chitosan composite nano-fiber membrane, and right figure is The SEM figures of gelatin/chitosan composite nano-fiber membrane after oxidized glucan crosslinking.It can be seen that passing through electrostatic Spin processes successfully prepare that surface is smooth and the homogeneous gelatin/chitosan composite nano-fiber membrane of diameter, and oxidized Portugal The fibre structure of gelatin/chitosan composite nano-fiber membrane is not substantially destroyed after glycan crosslinking.
Embodiment 2
(1) weigh 10.0g ferric trichlorides to be dissolved in the D/W that mass fraction is 20wt%, in the bar of lucifuge Reaction 24h is stirred vigorously under part under the conditions of 50 DEG C, reacted solution is dialysed 2 days, the solution after dialysis is chilled dry The dry glucose for being aoxidized;
(2) gelatin and shitosan are dissolved separately in the acetum of 90wt%, magnetic agitation, prepare quality point Number is the gelatin and chitosan solution of the transparent and homogeneous of 30wt% and 5wt%;
(3) by the gelatin and chitosan solution described in above-mentioned steps (2) with mass ratio be 9:1 ratio blending, stirs 2h Obtain the electrostatic spinning precursor liquid of transparent and homogeneous;
(4) the above-mentioned solution for preparing is fitted into syringe, and is fixed on the propeller of electrostatic spinning apparatus, passed through Electrostatic spinning prepares gelatin/chitosan composite nano-fiber membrane;The condition of wherein electrostatic spinning is as follows:Spinning temperature is 40 DEG C, Humidity is 60%, and fltting speed is 2.0mL/h, and voltage is 25kV, and the distance of spinning head to receiver board is 20cm;
(5) glucose by the oxidation prepared in step (1) is dissolved in absolute ethyl alcohol, takes a certain amount of step (4) the gelatin/chitosan composite nano-fiber membrane prepared in, the glucose for being cut into rectangle and being soaked in oxidation is handed over In connection medium, it is crosslinked 1 day under the conditions of 37 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
Fig. 2 is that embodiment 2 is obtained answering before and after the oxidized glucose of gelatin/chitosan composite nano-fiber membrane is crosslinked Force-strain curve.It can be seen that after oxidized glucose crosslinking Treatment, gelatin/chitosan composite nano-fiber membrane Mechanical property significantly increase.
Embodiment 3
(1) weigh 5.0g potassium metaperiodates to be dissolved in the carboxymethyl cellulose aqueous solution that mass fraction is 10%, in lucifuge Under conditions of be stirred vigorously under the conditions of 25 DEG C reaction 12h, by reacted solution dialyse 5 days, by the solution after dialysis through cold Jelly is dried to obtain the carboxymethylcellulose calcium of oxidation;
(2) gelatin and shitosan are dissolved separately in the acetum of 90wt%, magnetic agitation, prepare quality point Number is the gelatin and chitosan solution of the transparent and homogeneous of 10wt% and 15wt%;
(3) by above-mentioned polyelectrolyte solution with mass ratio be 5:5 ratio blending, stirring 5h obtains the electrostatic of transparent and homogeneous Spinning precursor liquid;
(4) the above-mentioned solution for preparing is fitted into syringe, and is fixed on the propeller of electrostatic spinning apparatus, passed through Electrostatic spinning prepares gelatin/chitosan composite nano-fiber membrane.The condition of wherein electrostatic spinning is as follows:Spinning temperature is 30 DEG C, Humidity is 30%, and fltting speed is 0.8mL/h, and voltage is 15kV, and the distance of spinning head to receiver board is 15cm;
(5) carboxymethylcellulose calcium by the oxidation prepared in step (1) is dissolved in absolute ethyl alcohol, is taken a certain amount of The gelatin/chitosan composite nano-fiber membrane prepared in step (4), is cut into rectangle and is soaked in the carboxylic first of oxidation In the cellulose crosslinked medium of base, it is crosslinked 4 days under the conditions of 37 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
Before Fig. 3 is oxidized carboxymethyl cellulose crosslinked of gelatin/chitosan composite nano-fiber membrane obtained in embodiment 3 Swelling behavior figure afterwards.It can be seen that the oxidized carboxymethylcellulose calcium of gelatin/chitosan composite nano-fiber membrane is handed over After connection, its swelling behavior is significantly reduced.
Embodiment 4
(1) weigh 0.5g potassium bichromates to be dissolved in the konjak portuguese gansu polyose sugar aqueous solution that mass fraction is 5%, in lucifuge Under the conditions of be stirred vigorously under the conditions of 15 DEG C reaction 10h, by reacted solution dialyse 2 days, the solution after dialysis is chilled It is dried to obtain the konjaku glucomannan of oxidation;
(2) gelatin and shitosan are dissolved separately in the acetum of 90wt%, magnetic agitation, prepare quality point Number is the gelatin and chitosan solution of the transparent and homogeneous of 20wt% and 5wt%;
(3) by above-mentioned polyelectrolyte solution with mass ratio be 7:3 ratio blending, stirring 4h obtains the electrostatic of transparent and homogeneous Spinning precursor liquid;
(4) the above-mentioned solution for preparing is fitted into syringe, and is fixed on the propeller of electrostatic spinning apparatus, passed through Electrostatic spinning prepares gelatin/chitosan composite nano-fiber membrane.The condition of wherein electrostatic spinning is as follows:Spinning temperature is 35 DEG C, Humidity is 30%, and fltting speed is 3.0mL/h, and voltage is 24kV, and the distance of spinning head to receiver board is 15cm;
(5) konjaku glucomannan by the oxidation prepared in step (1) is dissolved in absolute ethyl alcohol, is taken a certain amount of The gelatin/chitosan composite nano-fiber membrane prepared in step (4), is cut into rectangle and is soaked in the konjaku of oxidation In Glucomannan crosslinking medium, it is crosslinked 1 day under the conditions of 37 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
Fig. 4 is before the oxidized konjaku glucomannan of gelatin/chitosan composite nano-fiber membrane obtained in embodiment 4 is crosslinked Mass loss figure afterwards.It can be seen that the oxidized konjaku glucomannan of gelatin/chitosan composite nano-fiber membrane is handed over After connection, its water resistance is significantly improved.

Claims (5)

1. a kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane, includes following steps:
1) preparation of the biological polyoses of oxidation:
Weigh 0.1~10g strong oxidizers to be dissolved in the aqueous solution of 1~20wt% biological polyoses, under conditions of lucifuge acutely Stirring reaction, reacted solution is dialysed 1~5 day, the biological polyoses aoxidized after the solution after dialysis is freeze-dried;
2) preparation of gelatin/chitosan composite nano-fiber membrane:
Gelatin and shitosan are dissolved in acetum respectively, magnetic agitation, respectively obtain concentration for 5~30wt% is homogeneous Bright gelatin and chitosan solution, is then 1 with mass ratio:9~9:Two kinds of solution blendings, stirring are obtained homogeneous by 1 ratio Transparent electrostatic spinning precursor liquid, gelatin/chitosan is prepared by above-mentioned electrostatic spinning precursor liquid by method of electrostatic spinning again Composite nano-fiber membrane;
3) preparation of the gelatin/chitosan composite nano-fiber membrane of crosslinking:
By step 1) in the biological polyoses of oxidation that prepare be dissolved in absolute ethyl alcohol, take step 2) in prepare it is bright Glue/chitosan composite nano fibre film, is cut into small pieces and is soaked in the crosslinking medium of the biological polyoses of above-mentioned oxidation, 0 It is crosslinked 1~5 day under the conditions of~50 DEG C, the gelatin/chitosan composite nano-fiber membrane being crosslinked.
2. the crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane according to claim 1, it is characterised in that: Step 1) described in strong oxidizer be any one in potassium permanganate, sodium metaperiodate, potassium bichromate, potassium chlorate, ferric trichloride Or mixture.
3. the crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane according to claim 1, it is characterised in that: Step 1) described in biological polyoses be any one in glucan, konjaku glucomannan, carboxymethylcellulose calcium, glucose or mixed Compound.
4. the crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane according to claim 1, it is characterised in that: Step 1) described in reaction condition be 10~50 DEG C, the reaction time be 0.5~24h.
5. the crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane according to claim 1, it is characterised in that: Step 2) described in method of electrostatic spinning parameter it is as follows:Temperature is 10~60 DEG C, and humidity is 20~80%, and fltting speed is 0.1 ~3.0mL/h, voltage is 10~50kV, and the distance of spinning head to receiver board is 5~30cm.
CN201611270384.4A 2016-12-31 2016-12-31 A kind of crosslinking preparation method of gelatin/chitosan composite nano-fiber membrane Pending CN106758217A (en)

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CN112301542A (en) * 2020-10-20 2021-02-02 福建农林大学 Core-shell type composite nanofiber membrane and preparation method and application thereof
CN112760812A (en) * 2020-12-30 2021-05-07 中国热带农业科学院南亚热带作物研究所 Composite nanofiber membrane and preparation method and application thereof

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