CN109224115A - A kind of preparation method of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film - Google Patents
A kind of preparation method of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film Download PDFInfo
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- 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
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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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
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Abstract
The present invention relates to a kind of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film preparation methods.The different chitosan of grafting rate-oxidation microcrystalline cellulose is prepared into chitosan-oxidation microcrystalline cellulose medical biologic film of multilayer high porosity using casting filming therapy by coupling agent EDC and NHS by the present invention by chitosan and oxidation microcrystalline cellulose grafting.By the method for the two grafting film forming, the performance for the single raw material that both makes mutually to improve in performance obtains superior biological medicinal membrane.Present invention process process is simple, easy to operate and safe, mild condition；Medical biomembrane multilayer prepared by the present invention and high porosity, are able to respond the different phase of organization healing and play different functions, absorptive tissue diffusate, accelerate the diffusion transport of substance and the discharge of metabolin, keep wound moist, promote wound healing.
Description
Technical field
The invention belongs to functional polymer material fields, and in particular to a kind of chitosan-oxidation microcrystalline cellulose multilayer is high
The preparation method of porosity medical biologic film, obtained biofilm can be applied to the fields such as medicine, bioengineering.
Background technique
Chitosan is a kind of linear, semi-crystal shape basic natural polysaccharides macromolecule, have good biocompatibility and
Biological degradability, non-toxic, antibiotic property can promote cell to grow, suitable mild wet environment is provided for wound healing；It is ventilative
Property it is good, convenient for discharge wound exudate；It is resourceful, the features such as easy storage cheap and easy to get.In recent years, as modern Medical coating
The application of material receives great attention, is widely used in terms of antibiotic property, the promotion treatment such as wound healing and medicine controlled releasing.
However, due to their brittleness, pure chistosan film has poor mechanical performance, and which has limited its conducts under dampness
The use of wound dressing.
Aoxidizing microcrystalline cellulose is a kind of polymeric biomaterial, has nontoxic, biocompatibility, biological degradability and stops
The excellent characteristics such as courage and uprightness, certain carboxylic group is contained on strand, and reactivity is improved.Its mechanical strength simultaneously
Height, thermal stability is good, and dispersion performance is good, conducive to the stabilization of pharmaceutical preparation, has stronger suction to drug and other auxiliary ingredients
Attached effect, but be not easy to form a film.
Chitosan and oxidation microcrystalline cellulose are all biocompatibility and the excellent bio-medical material of biodegradable properties
Material, but the two has respective limitation.The present invention changes the two mutually in performance by the method for the two grafting film forming
Into improving the performance of single raw material, obtain superior biological medicinal membrane.
Summary of the invention
When the purpose of the present invention is for chitosan molecule and oxidation microcrystalline cellulose molecule respectively as medical dressing film
Existing shortcoming and existing chitosan one aoxidize microcrystalline cellulose and defect existing for preparation method are blended, and provide one kind
Easy to operate, preparation time is short, chitosan at low cost-oxidation microcrystalline cellulose multilayer high porosity medical biologic film system
Preparation Method.
The present invention is achieved through the following technical solutions above-mentioned purpose: being (1-3): 1 coupling agent with mass ratio
EDCHCL and NHS modification oxidation microcrystalline cellulose, by the chitosan of molecular weight 5-100 ten thousand, oxidation microcrystalline cellulose according to matter
Amount is than (1-2): 1 grafting film forming obtains chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film.
More specifically, using the method for following step:
(1) chitosan for weighing molecular weight 5-100 ten thousand is put into the HAC solution of 50.00mL2%, and magnetic force stirs at 65 DEG C
It mixes, makes it completely dissolved, weigh oxidation microcrystalline cellulose and be added in 50.00mL deionized water, N is filled in 40 DEG C of stirrings2Deoxygenation
30min, until being completely dissolved.Proportion (1-3): 1 EDCHCL and NHS, stirring are added into oxidation microcrystalline cellulose solution
Activate 30min；Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently, end of reaction adds
The NaOH solution for entering 2% keeps the neutral generation of solution presentation cotton-shaped, and products obtained therefrom for several times is washed with deionized, and centrifugation 10min turns
Speed is 3000r/min, is dried to obtain oxidation microcrystalline cellulose-chitosan；Chitosan and oxidation microcrystalline cellulose mass ratio are (1-
2): 1；
(2) oxidation microcrystalline cellulose-chitosan is weighed, is dissolved in 5% acetum, 65 DEG C of stirrings are until sufficiently completely
Dissolution is added glycerol 3-4d, is sufficiently stirred；
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming puts it into casting film-forming in air dry oven.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Further, it is 30-60 DEG C that air dry oven drying temperature is entered in the step (3).
Preferably, EDCHCL and NHS mass ratio is 2:1, and chitosan and oxidation microcrystalline cellulose mass ratio are 1:1.
EDC and NHS is nontoxic, the good coupling agent of biocompatibility.EDC chemical property is active, can make amino and carboxyl
Between form amido bond.EDC reacts the O- acylurea intermediate to be formed and can be reacted with amino by the carboxyl with compound,
Under the conditions of NHS is existing, O- acylurea intermediate can be converted to the NHS ester of amino reactivity, to greatly improve EDC Jie
The condensation reaction efficiency led improves grafting yield.The present invention is by coupling agent EDC and NHS, by chitosan and oxidation microcrystalline cellulose
Element grafting, is prepared into multilayer high porosity for the different chitosan of grafting rate-oxidation microcrystalline cellulose using casting filming therapy
Chitosan-oxidation microcrystalline cellulose medical biologic film.By the method for the two grafting film forming, change the two mutually in performance
Into improving the performance of single raw material, obtain superior biological medicinal membrane.
Further, it is contemplated that polystyrene has nontoxic, transparent feature, easily observation film-forming state, therefore uses polyphenyl
Ethylene is as mold material.
The present invention by adopting the above technical scheme, mainly has the advantage that (1) reaction raw materials and reagent are cheap and easy to get, work
Skill process is simple, easy to operate and safe, mild condition；(2) multilayer chitosan-oxidation microcrystalline cellulose film dressing is able to respond group
It knits the different phase of healing and plays different functions, absorptive tissue diffusate keeps wound moist, and hemostatic and antibacterial promotes wound
Mouth healing；(3) chitosan-oxidation microcrystalline cellulose film dressing has higher porosity, and the big material of porosity has as dressing
Conducive to moisture-inhibiting, ventilative, the diffusion transport of substance and metabolin discharge, it is possible to provide enough spaces retain Porcine HGF.
Detailed description of the invention
Fig. 1 is chitosan-oxidation microcrystalline cellulose medical biologic film FT-IR spectrogram；Wherein, (a) chitosan, (b)
Chitosan-oxidation microcrystalline cellulose medical biomembrane (c) aoxidizes microcrystalline cellulose；
Fig. 2 is chitosan-oxidation microcrystalline cellulose medical biologic film section electron microscope；
Fig. 3 is chitosan-oxidation microcrystalline cellulose medical biologic film surface topography electron microscope；
Fig. 4 film-forming temperature, grafting rate are to the influence of chitosan-oxidation microcrystalline cellulose medical biologic film porosity；
Fig. 5 is casting solution concentration, grafting rate to chitosan-oxidation microcrystalline cellulose medical biologic film porosity shadow
It rings.
Specific embodiment
The present invention is described in detail below by specific embodiment, but is not limited the scope of the invention.Unless otherwise specified, originally
Experimental method used by inventing is conventional method, and experiment equipment used, material, reagent etc. can chemically company be bought.
Embodiment 1
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.End of reaction is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.2g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 2
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.End of reaction is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 3
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.8g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 4
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 1.0g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 5
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 30 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 6
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 40 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 7
(1) the chitosan 0.5g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL 2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 2:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 42.4%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 42.4% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 60 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 8
(1) the chitosan 0.5g that molecular weight is 50000 is weighed, the HAC solution of 50.00mL2%, the magnetic force at 65 DEG C are put into
Stirring, makes it completely dissolved.It weighs 0.25g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 60 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 3:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 61.2%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 61.2% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 9
(1) the chitosan 0.25g that molecular weight is 200000 is weighed, the HAC solution of 50.00mL2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 1.0g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 40 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 3:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 28.2%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 28.2% is weighed, is dissolved in 5% acetum,
Until being sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for 65 DEG C of stirrings.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
Embodiment 10
(1) the chitosan 0.5g that molecular weight is 100000 is weighed, the HAC solution of 50.00mL2%, the magnetic at 65 DEG C are put into
Power stirring, makes it completely dissolved.It weighs 0.5g oxidation microcrystalline cellulose to be added in 50.00mL deionized water, 50 DEG C of stirrings are filled
N2Deoxygenation 30min, until being completely dissolved.The EDCHCL and NHS of 3:1 are added into oxidation microcrystalline cellulose solution, stirring is lived
Change 30min.Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently.Reflection finishes, and is added
2% NaOH solution makes solution that neutral generation be presented cotton-shaped.Products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan that grafting rate is 16%.
(2) oxidation microcrystalline cellulose-chitosan 0.5g that grafting rate is 16% is weighed, is dissolved in 5% acetum, 65
Until be sufficiently completely dissolved, addition glycerol 3-4d is sufficiently stirred for DEG C stirring.
(3) solution is poured into clean at curtain coating in bellows, is sprawled on polystyrene mould, in a vacuum drying oven
It is put into 1h, standing and defoaming.Casting film-forming in air dry oven is put it into, film-forming temperature is 50 DEG C.
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, every time
1h, until solution is in neutrality.
It is infrared that Fig. 1 compared chitosan, oxidation microcrystalline cellulose and chitosan-oxidation microcrystalline cellulose medical biomembrane
Spectrogram.It was found that in chitosan-oxidation microcrystalline cellulose medical biomembrane spectrogram, in 1616.06cm-1、1542cm-1It inhales at place
Peak is received, amide I, II bands of a spectrum of amido bond are belonged to, illustrates to aoxidize microcrystalline cellulose and chitosan at carboxyl and amino position
It is combined by forming amido bond.
Chitosan-oxidation microcrystalline cellulose medical biologic film section and table are measured through tengsten lamp scanning electron microscope
Face pattern amplifies 300 times of electron microscopes, as shown in Figures 2 and 3.
Fig. 4 and Fig. 5 is respectively film-forming temperature, casting solution concentration, grafting rate to chitosan-medical life of oxidation microcrystalline cellulose
The influence of object film porosity.From Fig. 4 and Fig. 5 it is found that porosity and chitosan-oxidation microcrystalline cellulose grafting rate and film forming
Temperature is closely related, its porosity reaches maximum when grafting rate is 42.4%.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (5)
1. a kind of chitosan-oxidation microcrystalline cellulose multilayer high porosity medical biologic film preparation method, which is characterized in that
It is (1-3) with mass ratio: 1 coupling agent EDCHCL and NHS modification oxidation microcrystalline cellulose, by the shell of molecular weight 5-100 ten thousand
Glycan, oxidation microcrystalline cellulose are according to mass ratio (1-2): it is high to obtain chitosan-oxidation microcrystalline cellulose multilayer for 1 grafting film forming
Porosity medical biologic film.
2. preparation method according to claim 1, which is characterized in that using the method for following step:
(1) chitosan for weighing molecular weight 5-100 ten thousand, is put into the HAC solution of 50.00mL 2%, and the magnetic agitation at 65 DEG C makes
It is completely dissolved, and weighs oxidation microcrystalline cellulose and is added in 50.00mL deionized water, and N is filled in 40 DEG C of stirrings2Deoxygenation 30min,
Until being completely dissolved；Proportion (1-3): 1 EDCHCL and NHS, stir-activating is added into oxidation microcrystalline cellulose solution
30min；Chitosan solution is added dropwise into above-mentioned solution, continues to stir 20h, reacts it sufficiently, end of reaction is added
2% NaOH solution keeps the neutral generation of solution presentation cotton-shaped, products obtained therefrom for several times is washed with deionized, is centrifuged 10min revolving speed
For 3000r/min, it is dried to obtain oxidation microcrystalline cellulose-chitosan；Chitosan and oxidation microcrystalline cellulose mass ratio are (1-
2): 1；
(2) oxidation microcrystalline cellulose-chitosan is weighed, is dissolved in 5% acetum, 65 DEG C of stirrings are until sufficiently completely molten
Solution is added glycerol 3-4d, is sufficiently stirred；
(3) solution is poured into clean at curtain coating in bellows, is sprawled on mold, is put into 1h in a vacuum drying oven, stands
Deaeration puts it into casting film-forming in air dry oven；
(4) film is used into NaOH aqueous solution soaking 30min, goes NaOH solution, for several times using distilled water immersion, each 1h, directly
It is in neutrality to solution.
3. preparation method according to claim 2, which is characterized in that enter the dry temperature of air dry oven in the step (3)
Degree is 30-60 DEG C.
4. preparation method according to claim 1, which is characterized in that EDCHCL and NHS mass ratio is 2:1, chitosan
It is 1:1 with oxidation microcrystalline cellulose mass ratio.
5. preparation method according to claim 2, which is characterized in that using polystyrene as mold material.
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| CN112175379A (en) * | 2020-09-30 | 2021-01-05 | 潘肖芬 | Biological membrane material |
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