CN109646703A - A kind of nano-cellulose composite antibacterial material and the preparation method and application thereof - Google Patents
A kind of nano-cellulose composite antibacterial material and the preparation method and application thereof Download PDFInfo
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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
- A61L15/22—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
- 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
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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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
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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
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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Abstract
The invention discloses a kind of nano-cellulose composite antibacterial materials and the preparation method and application thereof, prepare chitin quaternary ammonium salt/organic rectorite intercalation material QCR first, then it is compound with the progress of nano-cellulose CNFs foam.The composite material has excellent gas permeability, water imbibition, biocompatibility and antibiotic property etc., is used as medical dressing, can promote wound healing, and the bacteriostasis rate for Escherichia coli and staphylococcus aureus is 99.9% or more.
Description
Technical field
The present invention relates to a kind of nano-cellulose composite antibacterial materials and the preparation method and application thereof, belong to bio-medical material
Material field.
Background technique
The global skin injury as caused by tumble, burn, traffic accident, violence and war etc. every year be it is very common,
Wound is the main reason for leading to death, and wound surface poor healing influences whole world millions of people every year.Therefore, it selects
A kind of dressing that can effectively facilitate wound healing is very important.Skin wound healing is generally divided into four-stage: stopping blooding, disappears
Scorching, cell Proliferation and tissue reconstruction.Ideal Wound dressing should have haemostatic properties, have effective barrier action to microorganism,
Inflammatory reaction is low, can absorb wound exudate, keeps wet at the surface of a wound, promotes cell adherence and proliferation.It is cellulose nano-fibrous
It is a kind of material for being suitable for Wound dressing, because its good biocompatibility, large specific surface area, mechanical stability are good, causes people
Research interest.But cellulose does not have antibiotic property, so cellulose be usually pass through chemical modification or with other chemical combination
Object combines, and assigns its antibiotic property.
Chitin quaternary ammonium salt has excellent antibacterial effect, wherein positively charged quaternary ammonium salt group with it is negatively charged thin
Bacterium cell wall-bound destroys the barrier function of cell membrane, cytoplasm is caused to leak, eventually leads to bacterial death.Meanwhile chitin
Quaternary ammonium salt also has hydrophobic acetyl group, can promote it in conjunction with bacterial cell membrane lipid bilayer, more advantageous to antibacterial.By its
Intercalation material can be formed by ion exchange and rectorite by carrying out compound, positively charged polymer with rectorite or organic rectorite
Material, can be improved anti-microbial property, generally, rectorite interlamellar spacing is bigger, and antibiotic property is better.By this material load in cellulose
Nanofiber surface will be slow release intercalation material in use process, assigns nano cellulose material significant anti-microbial property, promotees
Into wound healing.
Summary of the invention
The purpose of the present invention is to provide a kind of for burning and the nano-cellulose of the Wound treatings such as wound is compound
The preparation method and application of anti-biotic material.
The present invention solves scheme used by above-mentioned technical problem and comprises the following specific steps that:
A kind of composite antibacterial material is obtained by chitin quaternary ammonium salt and organic rectorite intercalation synthesis.
Above-mentioned composite antibacterial material is prepared with the following method:
A) chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that mass fraction is 0.1%~0.5%；
B) in the chitin quaternary ammonium salt solution for obtaining organic rectorite addition step a), make organic rectorite and chitin
The mass ratio of quaternary ammonium salt is 1:1~1:20；
C) the obtained mixed liquor of step b) is heated to 60~90 DEG C, and continuously stirs 6~48h, be lyophilized, obtain after cooling
Chitin quaternary ammonium salt/organic rectorite intercalation material QCR.
Preferably, the mass ratio of organic rectorite and chitin quaternary ammonium salt is 1:0.5,1:1,1:2,1:5,1 in step b):
10,1:20, more preferably 1:5.
Preferably, the chitin quaternary ammonium salt is reacted by α-chitin or β-chitin with epoxypropyltrimethylchloride chloride
It is made, process includes: to be dispersed in α-chitin or β-chitin to be made of 8%NaOH, 4% urea, 88% distilled water
In mixed solution, wherein the mass ratio of α-chitin or β-chitin and mixed solution is 1:99.Freeze-thaw three times, obtains
The epoxypropyltrimethylchloride chloride for being 10:1 with α-chitin or β-chitin mass ratio is added at 15 DEG C in bright solution,
For 24 hours, dialysis to neutrality is lyophilized up to chitin quaternary ammonium salt for reaction.
The present invention also provides a kind of nano-cellulose composite antibacterial materials, by nano-cellulose carrier and are carried on therein
Anti-biotic material composition, wherein the anti-biotic material is above-mentioned composite antibacterial material or is obtained by above-mentioned preparation method compound anti-
Bacterium material QCR.
Above-mentioned nano-cellulose composite antibacterial material is prepared using following method:
(1) any one of composite antibacterial material described in claim 1 or claim 2~4 preparation method is obtained
Composite antibacterial material QCR is made into aqueous solution, and the nano-cellulose CNFs foam of freeze-drying is soaked in wherein, is taken out after a few hours,
Surface QCR solution is blotted with filter paper, is lyophilized compound up to nano-cellulose/chitin quaternary ammonium salt/organic rectorite CNFs/QCR
Material；
(2) composite material obtained by step (1) cut, encapsulated, ultraviolet irradiation disinfection is compound anti-to get CNFs/QCR
Bacterium material.
Preferably, the step of step (1) preparation CNFs/QCR composite material is as follows:
A) the nano-cellulose suspension that mass fraction is 0.1%~1% is lyophilized, obtains nano-cellulose CNFs bubble
Foam；
B) nano-cellulose CNFs foam is soaked in the QCR aqueous solution that mass fraction is 0.1%~1%, wherein receiving
The mass ratio of QCR is 1:2~10:1, preferably 1:1 in rice cellulose CNFs foam and solution, 12~48h is impregnated, by nanofiber
Element takes out from QCR solution, and the QCR solution of excess surface is sopped up with filter paper, is lyophilized again, obtains CNFs/QCR composite antibacterial material
Material.
Preferably, the nano-cellulose CNFs is made by TEMPO oxycellulose.Its process includes: to be by molar ratio
The TEMPO and NaBr of 1:1 is dissolved in distilled water, and cellulose is added, and NaClO solution is added, and adjusts reactant with NaOH solution
The pH of system is always 10 or so, until reaction terminates when NaOH is no longer consumed, remaining solid is washed with water after filtering to neutrality, residue is solid
Body is dispersed in water, ultrasound obtain it is cellulose nano-fibrous, 4 DEG C save it is stand-by.
The present invention also provides application of the above-mentioned nano-cellulose composite antibacterial material in biomedical materials field, are used as
Wound dressing, the bacteriostasis rate for Escherichia coli and staphylococcus aureus are 99.9% or more.
Composite material is made using cellulose nano-fibrous load chitin quaternary ammonium/organic rectorite for the first time in the present invention, this
A little composite materials have good anthemorrhagic performance and absorbability and excellent antibiotic property to wound exudate, and sustained release QCR is protected
Wound is protected not by bacteria attack, promotes collagen fibroblastic growth, accelerating wound healing.It is suitable for medical dressing, is applied to
Biomedical materials field.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained CNFs, QCR and CNFs/QCR of the embodiment of the present invention；In figure it is found that CNFs (a,
It d) is fibre structure, QCR (b, e) is unformed state, has many little particles on the fiber of CNFs/QCR (c, f), fiber also has
Thicker trend is that chitin quaternary ammonium salt/organic rectorite intercalation material is adhered on cellulose nano-fibrous；
Fig. 2 is that gained QC and QCR, can to the antibacterial effect of Escherichia coli, staphylococcus aureus in the embodiment of the present invention 1
Know, under same concentrations, QCR is better than QC to the antibacterial effect of Escherichia coli, staphylococcus aureus；
Fig. 3 is 1 gained CNFs/QCR and nano-cellulose CNFs of the embodiment of the present invention to Escherichia coli and golden yellow grape
The antibacterial effect of coccus, wherein Escherichia coli (a) and staphylococcus aureus (b)；It is found that cellulose nano-fibrous do not have in itself
Have an antibiotic property, but with chitin quaternary ammonium salt/organic rectorite intercalation material it is compound after have apparent antibiotic property；
Fig. 4 is the wound healing effect of 1 gained CNFs/QCR medical dressing and gauze of the embodiment of the present invention, wherein figure a, b,
C, d, e, f are the wound healing effect that the surface of a wound is applied using 1 gained dressing of the embodiment of the present invention；Scheming g, h, j, k, l, m is to use
The wound healing effect of the gauze application surface of a wound.
Specific embodiment
For a better understanding of the present invention, the following examples are to further explanation of the invention, but the contents of the present invention
It is not limited solely to the following examples.
Embodiment 1
Prepare chitin quaternary ammonium salt (QC)
0.016g TEMPO (1mmol) and 0.1g NaBr (1mmol) are dissolved in 100g distilled water, 1g fiber is added
7.5mL 5.2%NaClO solution is added in element, adjusts the pH of reaction system always 10 or so with the NaOH solution of 0.5mol/L,
Terminate to reaction when NaOH is no longer consumed, remaining solid is washed with water after filtering to neutrality, obtains chitin quaternary ammonium salt.
Prepare cellulose nano-fibrous (CNFs) foam
Cellulose is dispersed in water, 0.1% suspension, every 100mL suspension cell crushing instrument are configured to
(800w) ultrasound 10min obtains transparent nanofiber suspension, is concentrated to get the cellulose nanometer that concentration is 0.1%~1%
Fibrous suspension, freeze-drying, obtains cellulose nano-fibrous (CNFs) foam.
Chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that concentration is 0.5%；By organic rectorite plus
Enter in chitin quaternary ammonium salt solution, makes the mass ratio 1:5 of organic rectorite and chitin quaternary ammonium salt；Mixed liquor is heated to 90
DEG C, and continuously stirred for 24 hours at 90 DEG C, it is lyophilized after cooling, obtains QCR intercalation material, the QCR interlamellar spacing obtained under the ratio is most
Greatly, antibacterial effect is best.The CNFs foam that the cellulose nano-fibrous freeze-drying of 1000g 0.5% obtains is immersed in 1000g
In 0.5% QCR solution, impregnates for 24 hours, by cellulose nano-fibrous taking-up, the QCR solution of excess surface is sopped up with filter paper, then
Secondary freeze-drying obtains CNFs/QCR composite material.Composite material is cut, is encapsulated, ultraviolet irradiation sterilizes to get CNFs/QCR
Medical dressing.
Embodiment 2
Chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that concentration is 0.5%；By organic rectorite plus
Enter in chitin quaternary ammonium salt solution, makes the mass ratio 1:1 of organic rectorite and chitin quaternary ammonium salt；Mixed liquor is heated to 60
DEG C, and 48h is continuously stirred at 60 DEG C, it is lyophilized after cooling, obtains QCR intercalation material.1000g 1% is cellulose nano-fibrous
Obtained foam is lyophilized to be immersed in 1000g 0.1%QCR solution, impregnates 12h for cellulose nano-fibrous taking-up and uses filter paper
The QCR solution for sopping up excess surface, is lyophilized again, obtains CNFs/QCR composite material.
Embodiment 3
Chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that concentration is 0.25%；By organic rectorite
It is added in chitin quaternary ammonium salt solution, makes the mass ratio 1:10 of organic rectorite and chitin quaternary ammonium salt；Mixed liquor is heated
To 80 DEG C, and 12h is continuously stirred at 80 DEG C, be lyophilized after cooling, obtain QCR intercalation material.0.5% cellulose of 1000g is received
The foam that is lyophilized of rice fiber is immersed in 1000g 0.1%QCR solution, impregnates 12h, by cellulose nano-fibrous taking-up,
The QCR solution that excess surface is sopped up with filter paper, is lyophilized again, obtains CNFs/QCR composite material.
Embodiment 4
Chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that concentration is 0.1%；By organic rectorite plus
Enter in chitin quaternary ammonium salt solution, makes the mass ratio 1:20 of organic rectorite and chitin quaternary ammonium salt；Mixed liquor is heated to
60 DEG C, and 6h is continuously stirred at 60 DEG C, it is lyophilized after cooling, obtains QCR intercalation material.By 1% cellulose Nanowire of 1000g
The foam that dimension freeze-drying obtains is immersed in 1000g 0.5%QCR solution, 48h is impregnated, by cellulose nano-fibrous taking-up, with filter
Paper sops up the QCR solution of excess surface, is lyophilized again, obtains CNFs/QCR composite material.
Embodiment 5
Chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that concentration is 0.1%；By organic rectorite plus
Enter in chitin quaternary ammonium salt solution, makes the mass ratio 1:20 of organic rectorite and chitin quaternary ammonium salt；Mixed liquor is heated to
60 DEG C, and 6h is continuously stirred at 60 DEG C, it is lyophilized after cooling, obtains QCR intercalation material.By 0.5% cellulose nanometer of 1000g
The foam that fiber is lyophilized is immersed in 1000g 1%QCR solution, is impregnated for 24 hours, by cellulose nano-fibrous taking-up, with filter
Paper sops up the QCR solution of excess surface, is lyophilized again, obtains CNFs/QCR composite material.
Antibacterial effect evaluation
Antibacterial test, test result such as Fig. 2 and 3 institute are carried out to QC, QCR, CNFs/QCR composite material made from embodiment 1
Show.The operating procedure of Fig. 2: taking concentration is 5 × 106The bacterium solution of CFU/mL, 100 μ L bacterium solutions and the sample of 10mL various concentration are molten
Liquid mixes (sample concentration is between 1-100 μ g/mL), and 37 DEG C of shaking tables shake 10 hours, and mixed liquor is coated in LB (0.5% beef
Cream, 1% peptone, 1.5% agar, 0.5% sodium chloride, 96.5% water) on plate.37 DEG C of incubator cultures for 24 hours, observe plate
Upper colony counts, clump count is fewer, and antibacterial effect is better.The operating procedure of Fig. 3: taking concentration is 5 × 106The bacterium solution of CFU/mL,
100 μ L bacterium solutions are applied on LB plate, CNFs the and CNFs/QCRs foam that diameter is 6mm is attached to planar surface, 37 DEG C of cultures
Case culture for 24 hours, observes inhibition zone size, inhibition zone is bigger, and antibacterial effect is better.
Wound healing assay
Evaluate the promotion wound healing effect of dressing described in embodiment 1.As seen from the figure, obviously compared with the wound of CNFs/QCR
The wound of same period gauze wants small.Started to form a scab at the 9th day with the wound of CNFs/QCR, basic healing in the 12nd day.Due to gauze
There is no antibiotic property, have inflammatory reaction with the wound initial stage of gauze, start to form a scab with the 12nd talent of wound of gauze, heals completely
15 days are taken, therefore, effect 3 days faster than gauze of the promotion wound healing of dressing described in embodiment 1.
The more antibacterial effects of QCR are better, and when CNFs:QCR is 1:1, the bacteriostasis rate of composite material can achieve 99.9%
More than, it is little to the increase effect of bacteriostasis rate to continue growing QCR content, but QCR chance water is soluble, QCR is more, composite material
Intensity can decline.In order to make composite material have both intensity and antibiotic property, optimal CNFs:QCR is 1:1.
The above is a preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these, which improve and change, is also considered as protection scope of the present invention.
Claims (9)
1. a kind of composite antibacterial material, which is characterized in that the composite antibacterial material is by chitin quaternary ammonium salt and organic rectorite
Intercalation synthesis obtains.
2. the preparation method of composite antibacterial material as described in claim 1, which comprises the steps of:
A) chitin quaternary ammonium salt is dissolved in water, obtains the chitin quaternary ammonium salt solution that mass fraction is 0.1%~0.5%；
B) in the chitin quaternary ammonium salt solution for obtaining organic rectorite addition step a), make organic rectorite and chitin quaternary ammonium
The mass ratio of salt is 1:1~1:20；
C) the obtained mixed liquor of step b) is heated to 60~90 DEG C, and continuously stirs 6~48h, be lyophilized after cooling, obtain crust
Plain quaternary ammonium salt/organic rectorite intercalation material QCR.
3. preparation method according to claim 2, which is characterized in that organic rectorite and chitin quaternary ammonium salt in step b)
Mass ratio be 1:5.
4. preparation method according to claim 2, which is characterized in that the chitin quaternary ammonium salt is by α-chitin or β-first
Shell element is reacted with epoxypropyltrimethylchloride chloride to be made.
5. a kind of nano-cellulose composite antibacterial material, which is characterized in that the nano-cellulose composite antibacterial material is by nanometer
Cellulose carrier and it is carried on anti-biotic material therein composition, wherein the anti-biotic material is described in claim 1 compound anti-
The composite antibacterial material QCR that any one of bacterium material or claim 2~4 preparation method obtain.
6. the preparation method of nano-cellulose composite antibacterial material as claimed in claim 5, which is characterized in that including walking as follows
It is rapid:
(1) any one of composite antibacterial material described in claim 1 or claim 2~4 preparation method is obtained compound
Anti-biotic material QCR is made into aqueous solution, and the nano-cellulose CNFs foam of freeze-drying is soaked in wherein, is taken out after a few hours, with filter
Paper blots surface QCR solution, is lyophilized up to nano-cellulose/chitin quaternary ammonium salt/organic rectorite CNFs/QCR composite material；
(2) composite material obtained by step (1) cut, encapsulated, ultraviolet irradiation sterilizes to get CNFs/QCR composite antibacterial material
Material.
7. preparation method according to claim 6, which is characterized in that step (1) prepares the step of CNFs/QCR composite material
It is rapid as follows:
A) the nano-cellulose suspension that mass fraction is 0.1%~1% is lyophilized, obtains nano-cellulose CNFs foam；
B) nano-cellulose CNFs foam is soaked in the QCR aqueous solution that mass fraction is 0.1%~1%, wherein Nanowire
The mass ratio for tieing up QCR in element CNFs foam and solution is 1:2~10:1,12~48h of immersion, by nano-cellulose from QCR solution
Middle taking-up sops up the QCR solution of excess surface with filter paper, is lyophilized again, obtains CNFs/QCR composite antibacterial material.
8. preparation method according to claim 6, which is characterized in that the nano-cellulose CNFs is aoxidized fine by TEMPO
Dimension element is made.
9. nano-cellulose composite antibacterial material the answering in biomedical materials field as described in any one of claim 6~8
With, which is characterized in that it is used as wound dressing, the bacteriostasis rate for Escherichia coli and staphylococcus aureus is 99.9% or more.
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| CN110144124A (en) * | 2019-05-07 | 2019-08-20 | 华中科技大学 | A kind of composite material and its preparation and application of quaternized chitin and fibroin albumen |
| CN110144124B (en) * | 2019-05-07 | 2020-07-10 | 华中科技大学 | Composite material of quaternized chitin and silk fibroin and preparation and application thereof |
| CN111849018A (en) * | 2020-04-30 | 2020-10-30 | 中南大学 | Rectorite-based flame-retardant aerogel and preparation and application thereof |
| CN113651894A (en) * | 2021-08-18 | 2021-11-16 | 佛山(华南)新材料研究院 | Preparation method and application of amphoteric nanocellulose |
| CN113651894B (en) * | 2021-08-18 | 2022-07-29 | 佛山(华南)新材料研究院 | Preparation method and application of amphoteric nanocellulose |
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