CN107007865A - A kind of chitosan black phosphorus composite aquogel and preparation method thereof - Google Patents
A kind of chitosan black phosphorus composite aquogel and preparation method thereof Download PDFInfo
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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
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
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Abstract
The invention provides chitosan black phosphorus composite aquogel dressing of a kind of quick light dynamic pasteurization and preparation method thereof, comprise the following steps：S1, in deionized water and it is passed through protection gas argon gas by black phosphorus (BP) crystal powder is scattered, then ultrasonic under condition of ice bath, it is standby that finally centrifugation obtains the upper strata nanometer black phosphorus piece aqueous solution；S2, prepare aquagel；S3, prepare chitosan black phosphorus composite aquogel.Produced in preparation process without pernicious gas, it is economic and environment-friendly；Preparation method is simple, equipment investment is few, and consumption resource is few, and enforcement difficulty is small；Ten minutes antibiotic rates of composite aquogel illumination can reach more than 99%, good biocompatibility.
Description
Technical field
The present invention relates to biology medical material technical field, and in particular to a kind of chitosan of quick light dynamic pasteurization-black
Phosphorus composite aquogel dressing and preparation method thereof.
Background technology
Bio-medical material is the basis for studying artificial organs and medicine equipment, for being diagnosed, being treated to organism
Illness, surgical repair replace its disease damage tissue, organ or promote its function, and will not produce dysgenic material to organism
Material.It is used as bio-medical material, it should be non-toxic to human body, without sensitization, nonirritant, hereditary-less toxicity and non-carcinogenesis
Deng adverse reaction.
Some gouges in life, damage, abrade and surgical operation, high temperature, radiation and chemical reagent etc. are easy to make
Into skin injury, if carrying out treatment of wounds not in time can cause to be made by microorganism especially Escherichia coli and staphylococcus aureus
Into bacterium infection.In recent years, rapidly and effectively treat such wound and cause extensive concern, and it is quick
Sterilization be a crucial process.Aquagel can effectively kill bacterium due to positively charged, but this is made
Use process time long, also just because of this strong electropositive, cytotoxicity is also very big.
The content of the invention
In view of this, the invention provides a kind of chitosan-black phosphorus composite aquogel and preparation method thereof, its antibiotic property
High, photocatalytic is good, good biocompatibility, and technique is simple, equipment investment is few, resource consumption is few, without pernicious gas by-product produce
It is raw.
First aspect present invention provides a kind of chitosan-black phosphorus composite aquogel preparation method, and step includes：
S1, in deionized water and be passed through protective gas by black phosphorus crystal powder is scattered, then under condition of ice bath ultrasound 8~
12h, it is standby that finally centrifugation obtains the upper strata nanometer black phosphorus piece aqueous solution；
S2, dissolve chitosan in aqueous acetic acid, stir, then in adding aloe powder, poly- second two at 45~55 DEG C
Alcohol and glycerine, injected slurry volume concentration is 1~2% glutaraldehyde water solution after stirring, and is placed in after stirring 40~60 in baking oven
6~9h at DEG C, that is, be made aquagel；
S3, the aquagel for preparing step S2 be soaked in 10 in nanometer black phosphorus piece aqueous solution as carrier~
20min, obtains chitosan-black phosphorus composite aquogel.
Second aspect of the present invention provides a kind of chitosan-black phosphorus composite aquogel, the chitosan-black phosphorus compound water congealing
Glue is that black phosphorus nanometer sheet is supported on the composite aquogel obtained on the aquagel in network structure.
The beneficial effects of the invention are as follows：
(1) aquagel is prepared using glutaraldehyde as crosslinking agent, while without heating, no pernicious gas production
It is raw, it is economic and environment-friendly；
(2) preparation method is simple, equipment investment is few, and consumption resource is few, and enforcement difficulty is small；
(3) in composite aquogel dressing black phosphorus successful load, can not only strengthen photocatalytic so as to largely
Reduce cytotoxicity after improving antibacterial activity, and comprehensive hydrogel electropositive；
(4) composite aquogel antibiotic rate under illumination ten minutes can reach more than 99%, and with good biofacies
Capacitive.
Brief description of the drawings
Fig. 1 is the SEM figures of hydrogel in embodiment one；
Fig. 2 is the SEM figures of the black phosphorus piece loaded in embodiment one；
Fig. 3 is obtained product in embodiment one, embodiment two, embodiment three, example IV and embodiment five in illumination
Antibiotic rate block diagram after 10min.
Embodiment
First aspect present invention provides a kind of chitosan-black phosphorus composite aquogel preparation method, and step includes：
S1, in deionized water and be passed through protective gas by black phosphorus crystal powder is scattered, then under condition of ice bath ultrasound 8~
12h, it is standby that finally centrifugation obtains the upper strata nanometer black phosphorus piece aqueous solution；
S2, dissolve chitosan in aqueous acetic acid, stir, then in adding aloe powder, poly- second two at 45~55 DEG C
Alcohol and glycerine, injected slurry volume concentration is 1~2% glutaraldehyde water solution after stirring, and is placed in after stirring 40~60 in baking oven
6~9h at DEG C, that is, be made aquagel；
S3, the aquagel for preparing step S2 be soaked in 10 in nanometer black phosphorus piece aqueous solution as carrier~
20min, obtains chitosan-black phosphorus composite aquogel.
Active oxygen (ROS), including singlet oxygen, hydroxyl radical free radical, superoxide radical, are urged with semi-conducting material light
Change is closely related, while they also have very excellent antibiotic property.A kind of black phosphorus, new two-dimensional semiconductor material, has
Good photocatalytic.Meanwhile, black phosphorus is negatively charged, in this preparation method, and we utilize the elecrtonegativity and chitosan of black phosphorus
The electropositive of hydrogel, load black phosphorus piece is combined both on carrier, and chitosan-black phosphorus composite aquogel is made, makes
This water gel, which ties up to ten minutes lower antibiotic rates of illumination, can reach more than 99%, and with good biocompatibility.
It is preferred that, in step S1, every 40~60mg black phosphorus crystal powder is dispersed in 60~80mL deionized water.
More preferred, in step S1, the black phosphorus crystal powder per 50mg is dispersed in 80mL deionized water, then in ice
Ultrasound 8h under the conditions of bath.
More preferred, the rotating speed centrifuged described in step S1 is 1500r/min, and the time is 20min；It is ultrasonic described in step S1
Power be 1~1.5kW.
It is preferred that, in step S2, every 1~3g chitosans are dissolved in 100mL aqueous acetic acids, and stirring is then in 45~55
0.5~1.5g aloe powders, 1~3g polyethylene glycol and 1~3mL glycerine are sequentially added at DEG C, 20mL volumes are injected after stirring
Concentration is 1~2% glutaraldehyde.
More preferred, deacetylation >=95% of step S2 chitosans, viscosity is 100~200mPa.S, polyethylene glycol
Molecular weight is 2000.
Specifically, in several embodiments of the invention, in step S2, adding 5~10s of quick stirring after glutaraldehyde, soon
Pour into after mould and be placed in again in baking oven after speed stirring, the mould is a diameter of 15cm glass dish.
It is preferred that, it is water-soluble that the aquagel that every 1~3g chitosans are prepared is soaked in 1~2mL nanometers of black phosphorus pieces
In liquid.Specifically, in several embodiments of the invention, the disk that aquagel is cut into a diameter of 8mm is carried out again
Immersion treatment.
Second aspect of the present invention provides a kind of chitosan-black phosphorus composite aquogel, the chitosan-black phosphorus compound water congealing
Glue is that black phosphorus nanometer sheet is supported on the composite aquogel obtained on the aquagel in network structure.
It is preferred that, the chitosan-black phosphorus composite aquogel is prepared using aforementioned preparation process.
More preferred, the chitosan-black phosphorus composite aquogel is used as dressing.
A kind of chitosan-black phosphorus the composite aquogel provided below in conjunction with specific embodiment the present invention and its preparation side
Method is further described.The embodiments described below is exemplary, is only used for explaining the present invention, and it is not intended that to this
The limitation of invention.
Experimental method in following embodiments, is conventional method unless otherwise specified.Reality used in following embodiments
Test material unless otherwise specified, be that market is commercially available.
Embodiment one
S1, by 50mg black phosphorus (BP) crystal powder be dispersed in 80mL deionized water and be passed through protection gas argon gas, then
The ultrasound 10h under condition of ice bath, finally centrifuges the 20min acquisitions upper strata nanometer black phosphorus piece aqueous solution standby；
S2,2.5 chitosan is dissolved in the aqueous acetic acid that 100mL volumetric concentration is 2%, off line tool is not stirred
20min is mixed, in the water-bath for being subsequently placed in 50 DEG C, the glycerine of 1g aloe powder, 2g polyethylene glycol and 1mL is sequentially added,
Juxtaposition in mould is poured into after the glutaraldehyde water solution that 20mL volumetric concentrations are 2%, Quick mechanical stirring 5s are injected after stirring
Aquagel is made in 9h in 50 DEG C of baking ovens；
S3, the aquagel for preparing step S2 are soaked in the 2mL nanometer black phosphorus piece aqueous solution as carrier
15min, using the elecrtonegativity and the electropositive of aquagel of black phosphorus, load black phosphorus piece is on carrier, obtaining chitosan/black
Phosphorus composite aquogel.
Testing result is as follows to be detected to product obtained above：
As depicted in figs. 1 and 2, hydrogel shows the network structure of rule, and black phosphorus piece is supported on above hydrogel；
As shown in figure 3, the product of the preparation of embodiment one antibiotic rate block diagram after illumination 10min：To Escherichia coli antibacterial
Rate is 99.01%；It is 99.99% to staphylococcus aureus antibiotic rate.
Embodiment two
S1, by 40mg black phosphorus (BP) crystal powder be dispersed in 80mL deionized water and be passed through protection gas argon gas, then
The ultrasound 8h under condition of ice bath, finally centrifuges the 20min acquisitions upper strata nanometer black phosphorus piece aqueous solution standby；
S2,2g chitosan is dissolved in the aqueous acetic acid that 100mL volumetric concentration is 3%, off line tool is not stirred
15min is mixed, in the water-bath for being subsequently placed in 50 DEG C, the sweet of 0.5g aloe powder, 1g polyethylene glycol and 1mL is sequentially added
Oil, is poured into mould simultaneously after the glutaraldehyde water solution that 20mL volumetric concentrations are 1%, Quick mechanical stirring 6s are injected after stirring
It is placed in 6h in 40 DEG C of baking ovens and aquagel is made；
S3, the aquagel for preparing step S2 are soaked in the 1mL nanometers of black phosphorus piece aqueous solution as carrier
10min, using the elecrtonegativity and the electropositive of aquagel of black phosphorus, load black phosphorus piece is on carrier, obtaining chitosan/black
Phosphorus composite aquogel.
Testing result is as follows to be detected to product obtained above：
As shown in figure 3, the product of the preparation of embodiment two antibiotic rate block diagram after illumination 10min：To Escherichia coli antibacterial
Rate is 89.23%；It is 80.19% to staphylococcus aureus antibiotic rate.
Embodiment three
S1, by 60mg black phosphorus (BP) crystal powder be dispersed in 60mL deionized water and be passed through protection gas argon gas, then
The ultrasound 10h under condition of ice bath, finally centrifuges the 20min acquisitions upper strata nanometer black phosphorus piece aqueous solution standby；
S2,3g chitosan is dissolved in the aqueous acetic acid that 100mL volumetric concentration is 1%, off line tool is not stirred
30min is mixed, in the water-bath for being subsequently placed in 50 DEG C, the sweet of 1.5g aloe powder, 3g polyethylene glycol and 3mL is sequentially added
Oil, is poured into mould simultaneously after the glutaraldehyde water solution that 20mL volumetric concentrations are 3%, Quick mechanical stirring 8s are injected after stirring
It is placed in 9h in 60 DEG C of baking ovens and aquagel is made；
S3, the aquagel for preparing step S2 are soaked in the 2mL nanometers of black phosphorus piece aqueous solution as carrier
20min, using the elecrtonegativity and the electropositive of aquagel of black phosphorus, load black phosphorus piece is on carrier, obtaining chitosan/black
Phosphorus composite aquogel.
Testing result is as follows to be detected to product obtained above：
As shown in figure 3, the product of the preparation of embodiment three antibiotic rate block diagram after illumination 10min：To Escherichia coli antibacterial
Rate is 97.96%；It is 95.45% to staphylococcus aureus antibiotic rate.
Example IV
S1, by 50mg black phosphorus (BP) crystal powder be dispersed in 60mL deionized water and be passed through protection gas argon gas, then
The ultrasound 12h under condition of ice bath, finally centrifuges the 20min acquisitions upper strata nanometer black phosphorus piece aqueous solution standby；
S2,3g chitosan is dissolved in the aqueous acetic acid that 100mL volumetric concentration is 2.5%, not off line tool
Stir in 10min, the water-bath for being subsequently placed in 50 DEG C, sequentially add the sweet of 1g aloe powder, 2g polyethylene glycol and 1.5mL
Oil, injects the glutaraldehyde water solution that 20mL volumetric concentrations are 1.5%, 10s pours into mould after Quick mechanical stirring after stirring
In be placed in 50 DEG C of baking ovens 8h aquagel be made；
S3, the aquagel for preparing step S2 are soaked in the 1.5mL nanometers of black phosphorus piece aqueous solution as carrier
15min, using the elecrtonegativity and the electropositive of aquagel of black phosphorus, load black phosphorus piece is on carrier, obtaining chitosan/black
Phosphorus composite aquogel.
Testing result is as follows to be detected to product obtained above：
As shown in figure 3, the product of example IV preparation antibiotic rate block diagram after illumination 10min：To Escherichia coli antibacterial
Rate is 98.77%；It is 94.71% to staphylococcus aureus antibiotic rate.
Embodiment five
S1, by 55mg black phosphorus (BP) crystal powder be dispersed in 75mL deionized water and be passed through protection gas argon gas, then
The ultrasound 12h under condition of ice bath, finally centrifuges the 20min acquisitions upper strata nanometer black phosphorus piece aqueous solution standby；
S2,2.5g chitosan is dissolved in the aqueous acetic acid that 100mL volumetric concentration is 1.5%, not off line
Tool stirs 25min, in the water-bath for being subsequently placed in 50 DEG C, sequentially add 1.5g aloe powder, 1.5g polyethylene glycol and
2.5mL glycerine, falls after the glutaraldehyde water solution that 20mL volumetric concentrations are 2%, Quick mechanical stirring 7s are injected after stirring
Enter to be placed in 7h in 45 DEG C of baking ovens in mould and aquagel is made；
S3, the aquagel for preparing step S2 are soaked in the 1mL nanometers of black phosphorus piece aqueous solution as carrier
10min, using the elecrtonegativity and the electropositive of aquagel of black phosphorus, load black phosphorus piece is on carrier, obtaining chitosan/black
Phosphorus composite aquogel.
Testing result is as follows to be detected to product obtained above：
As shown in figure 3, for embodiment five prepare product after illumination 10min antibiotic rate block diagram：It is anti-to Escherichia coli
Bacterium rate is 91.42%；It is 87.51% to staphylococcus aureus antibiotic rate.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of chitosan-black phosphorus composite aquogel, it is characterised in that：Step includes：
S1, in deionized water and it is passed through protective gas by black phosphorus crystal powder is scattered, then 8~12h of ultrasound under condition of ice bath,
It is standby that finally centrifugation obtains the upper strata nanometer black phosphorus piece aqueous solution；
S2, dissolve chitosan in aqueous acetic acid, stir, then in added at 45~55 DEG C aloe powder, polyethylene glycol and
Glycerine, injected slurry volume concentration is 1~2% glutaraldehyde water solution after stirring, and is placed in after stirring in baking oven 6 at 40~60 DEG C
~9h, that is, be made aquagel；
S3, the aquagel for preparing step S2 are soaked in 10~20min in nanometer black phosphorus piece aqueous solution as carrier, obtain
Obtain chitosan-black phosphorus composite aquogel.
2. the preparation method of chitosan as claimed in claim 1-black phosphorus composite aquogel, it is characterised in that：In step S1, often
40~60mg black phosphorus crystal powder is dispersed in 60~80mL deionized water.
3. the preparation method of chitosan as claimed in claim 2-black phosphorus composite aquogel, it is characterised in that：In step S1, often
50mg black phosphorus crystal powder is dispersed in 80mL deionized water, then the ultrasound 8h under condition of ice bath.
4. the preparation method of chitosan as claimed in claim 2-black phosphorus composite aquogel, it is characterised in that：Described in step S1
The rotating speed of centrifugation is 1500r/min, and the time is 20min；Ultrasonic power described in step S1 is 1~1.5kW.
5. the preparation method of chitosan as claimed in claim 1-black phosphorus composite aquogel, it is characterised in that：In step S2, often
1~3g chitosans are dissolved in 100mL aqueous acetic acids, stirring and then in sequentially adding 0.5~1.5g aloes at 45~55 DEG C
Powder, 1~3g polyethylene glycol and 1~3mL glycerine, inject the glutaraldehyde that 20mL volumetric concentrations are 1~2% after stirring.
6. the preparation method of chitosan as claimed in claim 5-black phosphorus composite aquogel, it is characterised in that：Step S2 shells gather
Deacetylation >=95% of sugar, viscosity is 100~200mPa.S, and molecular weight polyethylene glycol is 2000.
7. the preparation method of chitosan as claimed in claim 1-black phosphorus composite aquogel, it is characterised in that：Every 1~3g shells gather
The aquagel that sugar is prepared is soaked in the 1~2mL nanometers of black phosphorus piece aqueous solution.
8. a kind of chitosan-black phosphorus composite aquogel, it is characterised in that：The chitosan-black phosphorus composite aquogel is received for black phosphorus
Rice piece is supported on the composite aquogel obtained on the aquagel in network structure.
9. chitosan as claimed in claim 8-black phosphorus composite aquogel, it is characterised in that：The chitosan-black phosphorus Compound Water
Gel is prepared using the method described in any one of claim 1 to 7 claim.
10. chitosan as claimed in claim 9-black phosphorus composite aquogel, it is characterised in that：Chitosan-the black phosphorus is combined
Hydrogel is used as dressing.
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| CN108042565A (en) * | 2017-11-02 | 2018-05-18 | 深圳先进技术研究院 | A kind of black phosphorus nano material with antibiotic effect and preparation method thereof |
| CN108144059A (en) * | 2017-11-30 | 2018-06-12 | 中南大学 | A kind of two dimension black phosphorus nanometer sheet loading nano silvery composite material and preparation method thereof and the application as antibacterial agent |
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| WO2019095752A1 (en) * | 2017-11-15 | 2019-05-23 | 深圳大学 | Cellulose/black phosphorus nanosheet composite hydrogel and preparation method therefor |
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| CN110090307A (en) * | 2019-06-04 | 2019-08-06 | 中国科学院深圳先进技术研究院 | A kind of load medicine black phosphorus chitosan composite Nano ball and its preparation method and application |
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| CN113198042A (en) * | 2021-04-25 | 2021-08-03 | 华南理工大学 | Growth factor loaded injectable nanocomposite hydrogel material and construction method and application thereof |
| CN113181421A (en) * | 2021-05-12 | 2021-07-30 | 广州贝奥吉因生物科技股份有限公司 | Hydrogel wound dressing with antibacterial and immunoregulation functions and preparation method thereof |
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| CN113289053B (en) * | 2021-05-12 | 2022-05-20 | 广州贝奥吉因生物科技股份有限公司 | Antibacterial hydrogel wound dressing loaded with two-dimensional material and nanoparticles and preparation method thereof |
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| CN116271205A (en) * | 2023-03-30 | 2023-06-23 | 福州大学 | Liquid band-aid containing black phosphorus nano sheet component and preparation method thereof |
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