CN106832437B - A kind of preparation method of silver-carrying nano cellulose-chitosan complex film - Google Patents
A kind of preparation method of silver-carrying nano cellulose-chitosan complex film Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of silver-carrying nano cellulose-chitosan complex film, include the following steps: in nano-cellulose solution be added sodium metaperiodate be protected from light stirring, be centrifuged wash after obtain dialdehyde-based nano-cellulose；It adds new saturation silver ammino solution of matching and prepares silver-carrying nano cellulose；It is mixed to get silver-carrying nano cellulose-chitosan bacteriostatic film with chitosan solution.The nano-Ag particles prepared in the present invention are distributed in the network structure of dialdehyde-based nano-cellulose, very good solution nano silver problem easy to reunite；And preparation process does not need not needing to reduce production cost using chemical reducing agent using specific apparatus yet.The present invention improves the low problem of chitosan film mechanical strength using the preferable mechanical property of nano-cellulose, and the bacteriostasis property of chitosan film is improved further through load silver operation.Gained silver-carrying nano cellulose-chitosan complex film has broad application prospects in the industries such as antibacterial wound dressing and food packaging.
Description
Technical field
The present invention relates to antibacterial material preparation fields, and in particular to a kind of silver-carrying nano cellulose-chitosan complex film
Preparation method.
Background technique
Nano silver (Ag) has many advantages, such as that sterilizing ability is strong, activity is high, permeability is strong and is widely used in biomaterial suppression
Bacterium, medical material be antibacterial and the fields such as food packaging.The antibacterial efficiency of Ag is determined that i.e. nano Ag particles radius is got over by silver granuel diameter
Small, antibacterial efficiency is higher, but nanoparticle radius is smaller, and surface can be bigger, more easy to reunite in solution medium, limits and receives
The antibacterial efficiency of rice Ag.Nanometer Ag is supported on to specific surface area is larger, on the stable carrier of chemical property, not only can solve and receive
Problem rice Ag easy to reunite, can also control Ag particle diameter.The preparation method of nano silver has photoreduction met hod, electrochemical process at present
With chemical reduction method etc., photoreduction met hod and electrochemical process operation are more complex, need using specialized equipment, chemical reduction method needs make
It is at high cost with chemical reducing agent.Therefore it needs to develop the new nano silver preparation method of one kind and overcomes the problems, such as that above-mentioned technology exists,
Original position synthesizing nano-silver particle is a kind of feasible new method in the network of nano-cellulose.
Nano-cellulose (NCC) is that a kind of length is plain for the rod-like fibre of dozens to a few hundred nanometers, has high-crystallinity, height
It is other to be often used as reinforcing fiber modification for the characteristics such as Young's modulus, high intensity, degradable, bio-compatible, excellent in mechanical performance
Material, to obtain the excellent composite material of mechanical performance.It can be in cellulosic molecule by sodium metaperiodate selective oxidation cellulose
Aldehyde functions are introduced in structure, and redox reaction, Jin Er are occurred using the aldehyde radical in silver ammino solution and oxycellulose
Synthesizing nano-silver particle in situ, it is easy to reunite to solve its using nano-cellulose loading nano silvery in the network structure of nano-cellulose
The problem of.
It is further that silver-carrying nano cellulose (Ag/DNCC) and CS is compound, both played the excellent mechanical of nano-cellulose
The mechanical strength of CS film can be improved, and can assign CS film higher bacteriostasis property.Silver-Chitosan Composites patent report at present
There are many road, and in terms of the emphasis of research all concentrates on the bacteriostasis property of composite material, current patent is without research composite membrane
Mechanical strength.This patent utilizes the network structure loading nano silvery particle of nano-cellulose, avoids nano silver and oxidation occurs instead
The biocidal property of nano silver is answered, improved, and takes full advantage of the intermolecular hydrogen bonding that nano-cellulose and CS are formed and improves composite membrane
Mechanical strength, be conducive to expand silver-carrying nano cellulose-chitosan (Ag/DNCC-CS) composite membrane answering as antibacterial material
Use field.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of preparation method of silver-carrying nano cellulose-chitosan complex film, benefit
Nano silver is loaded with nano-cellulose, solves the problems, such as that nano silver is easy to reunite；Utilize the mechanics that nano-cellulose is excellent
The crisp frangible disadvantage of improved strength chitosan film film, while passing through the bacteriostasis property of loading nano silvery raising chitosan film.
To achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of preparation method of silver-carrying nano cellulose-chitosan complex film, includes the following steps:
S1, nano-cellulose is prepared
1g microcrystalline cellulose is added in ultrasonic cell disintegration cup and 100ml distilled water is ultrasonically treated, ultrasonic power
For 1500W, ultrasonic time 0.5h, standing takes upper layer suspension to obtain powdered receive through rotary evaporation concentration, freeze-drying
Rice cellulose (NCC)；
S2, preparation dialdehyde-based nano-cellulose
The resulting nano-cellulose powder 1g of step S1 is taken, is dissolved in 100ml distilled water and forms 1% (m/v) NCC suspension
1g sodium metaperiodate magnetic agitation under the conditions of being protected from light is added in liquid, using high speed centrifugation, after ultrasonic disperse, stands, takes upper layer outstanding
Supernatant liquid is concentrated through rotary evaporation, freeze-drying obtains the powdered nano-cellulose (DNCC) with dialdehyde based structures；
S3, silver-carrying nano cellulose is prepared
The resulting dialdehyde-based nano-cellulose powder 0.1g of step S2 is taken, 0.2% (m/v) of formation in 50ml distilled water is dissolved in
Suspension adds newly with saturation silver ammino solution, is sufficiently mixed and is placed in water-bath, obtains brown color suspension, and standing takes
Layer suspension obtains powdered silver-carrying nano cellulose (Ag/DNCC) through rotary evaporation concentration, freeze-drying；
S4, the resulting silver-carrying nano cellulose magnetic agitation 1h in deionized water of step S3 is weighed, dissolves it sufficiently
Form the Ag/DNCC suspension of 0.1%-0.5% (m/v)；It weighs 2g chitosan (CS) and is dissolved in 100ml, 2% under the conditions of 25 DEG C
(v/v) magnetic agitation 3h in acetum forms the chitosan-acetic acid solution of 2% (m/v)；
S5, by Ag/DNCC suspension obtained in step S4 according to 3%, 5% and 10% (w/w) and 0.4g of CS dry weight
Glycerol is added to together in the resulting chitosan-acetic acid solution of step S4, and magnetic agitation forms homogeneous solution, ultrasonic disperse, vacuum
Mixed solution is cast on polyfluortetraethylene plate after deaeration, in a vacuum drying oven in 45 DEG C of dry 72h, film is taken off and obtains carrying silver
Nano-cellulose-chitosan (Ag/DNCC-CS) composite membrane, the silver-carrying nano cellulose-chitosan complex film film thickness being prepared
It is 30-50 μm.
Preferably, nano-cellulose described in step S1 be rodlike, spherical or ellipsoid, length 30-200nm, directly
Diameter is 20-40nm.
Preferably, magnetic stirring speed described in step S2 is 12000r/min, and mixing time is centrifugation time for 24 hours
It is 10min/ times, centrifugal rotational speed 10000r/min, centrifugally operated 5-6 times, ultrasonic disperse power is 600W, and ultrasonic time is
30min。
Preferably, silver ammino solution dosage is newly matched described in step S3 is 2ml, and bath temperature is 40 DEG C, and water bath time is
20min, the silver-carrying nano cellulose being prepared are spherical or ellipsoid, diameter 20-30nm.
Preferably, chitosan described in step S4 be molecular weight 600000-800000, viscosity 500-2000mPas,
Deacetylation > 88%.
Preferably, magnetic stirring speed described in step S5 is 6000r/min, mixing time 2h, ultrasonic disperse function
Rate is 600W, and ultrasonic time 30min, the vacuum degree of vacuum degasing machine is -0.9MPa.
The invention has the following advantages:
(1) present invention reacts in situ in nano-cellulose network structure with silver ammino solution using dialdehyde-based nano-cellulose
Synthesizing nano-silver particle does not need not needing using equipment such as irradiation, microwaves using chemical reducing agent, preparation process green, ring
It protects, energy conservation, meets the requirement of Green Chemistry；
(2) nano-Ag particles that the present invention is prepared stably dispersing, not easy to reunite, nanometer in nano-cellulose system
Argent grain is spherical or ellipsoid, diameter 20-30nm；
(3) composite membrane that the present invention is prepared only relies on hydroxyl and chitosan present on nano-cellulose molecular structure
Imino group present on molecular structure combines under blending and forms hydrogen bond, and preparation process is simple, easy to operate；
(4) present invention solve the problems, such as chitosan film film it is crisp it is frangible, mechanical strength is poor, chitosan is not carried out complicated
Modified operation, but the mechanical strength for utilizing nano-cellulose excellent improves the mechanical property of chitosan film；
(5) present invention improves the bacteriostasis property of chitosan film by the way that nano silver is added in chitosan.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of silver-carrying nano cellulose in the embodiment of the present invention.
Fig. 2 is silver-carrying nano cellulose-chitosan complex film bacteriostasis property schematic diagram in the embodiment of the present invention.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment 1
S1, nano-cellulose is prepared
1g microcrystalline cellulose is added in ultrasonic cell disintegration cup and 100ml distilled water is ultrasonically treated, ultrasonic power
For 1500W, ultrasonic time 0.5h, standing takes upper layer suspension to obtain powdered receive through rotary evaporation concentration, freeze-drying
Rice cellulose (NCC)；
S2, preparation dialdehyde-based nano-cellulose
Above-mentioned nano-cellulose powder 1g is taken, 1% (m/v) NCC suspension of formation in 100ml distilled water is dissolved in, 1g is added
Sodium metaperiodate under the conditions of being protected from light magnetic agitation, using high speed centrifugation, ultrasonic disperse, finally stand take upper layer suspension through revolving
Turn evaporation and concentration, freeze-drying obtains the powdered nano-cellulose (DNCC) with dialdehyde based structures；
S3, silver-carrying nano cellulose is prepared
Above-mentioned dialdehyde-based nano-cellulose powder 0.1g is taken, 0.2% (m/v) suspension of formation in 50ml distilled water is dissolved in,
It adds newly with saturation silver ammino solution, is sufficiently mixed and is placed in water-bath, obtain brown color suspension, standing takes upper layer suspension
Powdered silver-carrying nano cellulose (Ag/DNCC) is obtained through rotary evaporation concentration, freeze-drying；
S4, the silver-carrying nano cellulose prepared in step S3 magnetic agitation 1h in deionized water is weighed, keeps it sufficiently molten
Solution forms the Ag/DNCC suspension of 0.1% (m/v)；It weighs 2g chitosan (CS) and is dissolved in 100ml, 2% (v/ under the conditions of 25 DEG C
V) magnetic agitation 3h in acetum forms the chitosan-acetic acid solution of 2% (m/v)；
S5, by Ag/DNCC suspension obtained in step S4 according to 3%, 5% and 10% (w/w) and 0.4g of CS dry weight
Glycerol is added to together in CS solution, and mixed solution is cast by magnetic agitation after forming homogeneous solution, ultrasonic disperse, vacuum defoamation
In on polyfluortetraethylene plate, in a vacuum drying oven in 45 DEG C of dry 72h, takes off film and obtain silver-carrying nano cellulose-chitosan
(Ag/DNCC-CS) composite membrane.
Embodiment 2
S1, nano-cellulose is prepared
1g microcrystalline cellulose is added in ultrasonic cell disintegration cup and 100ml distilled water is ultrasonically treated, ultrasonic power
For 1500W, ultrasonic time 0.5h, standing takes upper layer suspension to obtain powdered receive through rotary evaporation concentration, freeze-drying
Rice cellulose (NCC)；
S2, preparation dialdehyde-based nano-cellulose
Above-mentioned nano-cellulose powder 1g is taken, 1% (m/v) NCC suspension of formation in 100ml distilled water is dissolved in, 1g is added
Sodium metaperiodate under the conditions of being protected from light magnetic agitation, using high speed centrifugation, ultrasonic disperse, finally stand take upper layer suspension through revolving
Turn evaporation and concentration, freeze-drying obtains the powdered nano-cellulose (DNCC) with dialdehyde based structures；
S3, silver-carrying nano cellulose is prepared
Above-mentioned dialdehyde-based nano-cellulose powder 0.1g is taken, 0.2% (m/v) suspension of formation in 50ml distilled water is dissolved in,
It adds newly with saturation silver ammino solution, is sufficiently mixed and is placed in water-bath, obtain brown color suspension, standing takes upper layer suspension
Powdered silver-carrying nano cellulose (Ag/DNCC) is obtained through rotary evaporation concentration, freeze-drying；
S4, the silver-carrying nano cellulose prepared in step S3 magnetic agitation 1h in deionized water is weighed, keeps it sufficiently molten
Solution forms the Ag/DNCC suspension of 0.3% (m/v)；It weighs 2g chitosan (CS) and is dissolved in 100ml, 2% (v/ under the conditions of 25 DEG C
V) magnetic agitation 3h in acetum forms the chitosan-acetic acid solution of 2% (m/v)；
S5, by Ag/DNCC suspension obtained in step S4 according to 3%, 5% and 10% (w/w) and 0.4g of CS dry weight
Glycerol is added to together in CS solution, and mixed solution is cast by magnetic agitation after forming homogeneous solution, ultrasonic disperse, vacuum defoamation
In on polyfluortetraethylene plate, in a vacuum drying oven in 45 DEG C of dry 72h, takes off film and obtain silver-carrying nano cellulose-chitosan
(Ag/DNCC-CS) composite membrane.
Embodiment 3
S1, nano-cellulose is prepared
1g microcrystalline cellulose is added in ultrasonic cell disintegration cup and 100ml distilled water is ultrasonically treated, ultrasonic power
For 1500W, ultrasonic time 0.5h, standing takes upper layer suspension to obtain powdered receive through rotary evaporation concentration, freeze-drying
Rice cellulose (NCC)；
S2, preparation dialdehyde-based nano-cellulose
Above-mentioned nano-cellulose powder 1g is taken, 1% (m/v) NCC suspension of formation in 100ml distilled water is dissolved in, 1g is added
Sodium metaperiodate under the conditions of being protected from light magnetic agitation, using high speed centrifugation, ultrasonic disperse, finally stand take upper layer suspension through revolving
Turn evaporation and concentration, freeze-drying obtains the powdered nano-cellulose (DNCC) with dialdehyde based structures；
S3, silver-carrying nano cellulose is prepared
Above-mentioned dialdehyde-based nano-cellulose powder 0.1g is taken, 0.2% (m/v) suspension of formation in 50ml distilled water is dissolved in,
It adds newly with saturation silver ammino solution, is sufficiently mixed and is placed in water-bath, obtain brown color suspension, standing takes upper layer suspension
Powdered silver-carrying nano cellulose (Ag/DNCC) is obtained through rotary evaporation concentration, freeze-drying；
S4, the silver-carrying nano cellulose prepared in step S3 magnetic agitation 1h in deionized water is weighed, keeps it sufficiently molten
Solution forms the Ag/DNCC suspension of 0.5% (m/v)；It weighs 2g chitosan (CS) and is dissolved in 100ml, 2% (v/ under the conditions of 25 DEG C
V) magnetic agitation 3h in acetum forms the chitosan-acetic acid solution of 2% (m/v)；
S5, by Ag/DNCC suspension obtained in step S4 according to 3%, 5% and 10% (w/w) and 0.4g of CS dry weight
Glycerol is added to together in CS solution, and mixed solution is cast by magnetic agitation after forming homogeneous solution, ultrasonic disperse, vacuum defoamation
In on polyfluortetraethylene plate, in a vacuum drying oven in 45 DEG C of dry 72h, takes off film and obtain silver-carrying nano cellulose-chitosan
(Ag/DNCC-CS) composite membrane.
The transmission electron microscope of silver-carrying nano cellulose is as shown in Figure 1；The load silver that content of nanometer silver is 0.5% under optimum condition is received
Rice cellulose-chitosan complex film bacteriostasis property is as shown in Figure 2；Silver-carrying nano cellulose-chitosan complex film mechanical property
As shown in table 1.
1 silver-carrying nano cellulose of table-chitosan complex film mechanical property
In conclusion this specific implementation does not need not needed chemical reducing agent using equipment such as irradiation, microwaves and only passed through two
Aldehyde radical nano-cellulose and silver ammino solution synthesizing nano-silver particle, pass through nano-cellulose loading nano silvery, very good solution
The agglomeration traits of nano silver.The preparation of composite membrane only relies on natural reaction, is not necessarily to special preparation technique, simple to operation；Pass through
The excellent mechanical performance effective solution of the nano-cellulose problem of chitosan film mechanical strength difference, is improved by carrying nano silver
The bacteriostasis property of chitosan film.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film, which comprises the steps of:
S1, nano-cellulose is prepared
1g microcrystalline cellulose is added in ultrasonic cell disintegration cup and 100ml distilled water is ultrasonically treated, ultrasonic power is
1500W, ultrasonic time 0.5h, standing take upper layer suspension to obtain powdered nanometer through rotary evaporation concentration, freeze-drying
Cellulose (NCC)；
S2, preparation dialdehyde-based nano-cellulose
The resulting nano-cellulose powder 1g of step S1 is taken, formation 1%NCC suspension in 100ml distilled water is dissolved in, 1g high is added
Sodium iodate magnetic agitation under the conditions of being protected from light after ultrasonic disperse, is stood, takes upper layer suspension through rotating using high speed centrifugation
It is concentrated by evaporation, freeze-drying obtains the powdered nano-cellulose (DNCC) with dialdehyde based structures；
S3, silver-carrying nano cellulose is prepared
The resulting dialdehyde-based nano-cellulose powder 0.1g of step S2 is taken, is dissolved in 50ml distilled water and forms 0.2% suspension, then
It is added newly with saturation silver ammino solution, is sufficiently mixed and is placed in water-bath, obtain brown color suspension, standing takes upper layer suspension to pass through
Rotary evaporation concentration, freeze-drying obtain powdered silver-carrying nano cellulose (Ag/DNCC)；″
S4, the resulting silver-carrying nano cellulose magnetic agitation 1h in deionized water of step S3 is weighed, it is made sufficiently to dissolve formation
The Ag/DNCC suspension of 0.1%-0.5%；Weigh 2g chitosan (CS) be dissolved under the conditions of 25 DEG C 100ml, 2% acetic acid it is molten
Magnetic agitation 3h in liquid forms 2% chitosan-acetic acid solution；
S5, weigh Ag/DNCC suspension obtained in step S4 according to 3%, the 5% of CS dry weight and 10%, then respectively with 0.4g
Glycerol is added in chitosan-acetic acid solution obtained in step S4, and it is de- that magnetic agitation forms homogeneous solution, ultrasonic disperse, vacuum
Mixed solution is cast on polyfluortetraethylene plate after bubble, in a vacuum drying oven in 45 DEG C of dry 72h, film is taken off and obtains load silver and receive
Rice cellulose-chitosan (Ag/DNCC-CS) composite membrane.
2. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film according to claim 1, feature exist
In: nano-cellulose described in step S1 is rodlike, spherical or ellipsoid, length 30-200nm, diameter 20-40nm.
3. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film according to claim 1, feature exist
In: magnetic stirring speed described in step S2 is 12000r/min, and mixing time is that for 24 hours, centrifugation time is 10min/ times, from
Heart revolving speed is 10000r/min, and centrifugally operated 5-6 times, ultrasonic disperse power is 600W, ultrasonic time 30min.
4. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film according to claim 1, feature exist
In: newly matching silver ammino solution dosage described in step S3 is 2ml, and bath temperature is 40 DEG C, and water bath time 20min is prepared into
The silver-carrying nano cellulose arrived is spherical or ellipsoid, diameter 20-30nm.
5. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film according to claim 1, feature exist
In: chitosan described in step S4 is molecular weight 600000-800000, viscosity 500-2000mPas, deacetylation >
88%.
6. a kind of preparation method of silver-carrying nano cellulose-chitosan complex film according to claim 1, feature exist
In: magnetic stirring speed described in step S5 is 6000r/min, and mixing time 2h, ultrasonic disperse power is 600W, ultrasound
Time is 30min, and the vacuum degree of vacuum degasing machine is -0.9MPa, the silver-carrying nano cellulose-chitosan complex film being prepared
Film thickness is 30-50 μm.
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