CN105999409A - Nano-antibacterial coating preparation method based on quaternized chitosan half-bred micelles - Google Patents
Nano-antibacterial coating preparation method based on quaternized chitosan half-bred micelles Download PDFInfo
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- CN105999409A CN105999409A CN201610576874.0A CN201610576874A CN105999409A CN 105999409 A CN105999409 A CN 105999409A CN 201610576874 A CN201610576874 A CN 201610576874A CN 105999409 A CN105999409 A CN 105999409A
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Abstract
The invention relates to a nano-antibacterial coating preparation method based on quaternized chitosan half-bred micelles. The preparation method includes the steps that firstly, quaternized chitosan is dissolved in 1% glacial acetic acid water solution to obtain a quaternized chitosan solution, then L-cysteine is dissolved in water to prepare an L-cysteine water solution, the two prepared solutions are mixed, a certain amount of solid nanozinc oxide is added, continuous stirring is performed, a pH value of the solution is regulated to promote system self-assembly after even mixing, and a half-bred micelle solution is obtained; finally, the half-bred micelle solution is used as electrolytic solution, the half-bred micelles are fixed to the medical metal surface by combining with an electrophoretic deposition technology to form a nano antibacterial coating. The nano-antibacterial coating preparation method is simple and convenient to operate, low in cost and wide in application range.
Description
Technical field
The present invention relates to a kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, belong to natural polymer
Combine field with antimicrobial coating, be also organic with inorganic hybridization system simultaneously.
Technical background
Research shows, forming antimicrobial coating has good inhibitory action on orthopaedics implant surface to bacterial adhesion and biofilm formation,
New research direction is provided for clinical prevention orthopaedics implant postoperative infection.The lotus positive electricity that chitosan uniquely exists as nature
Poly-polysaccharide, it has the anti-microbial property of excellence, but it only could obtain good solubility property and antibacterial effect in acid condition
Really, bacteriostasis is by a definite limitation.Chitosan quaternary ammonium salt not only has the character of typical quaternary ammonium salt by contrast, as antibacterial,
Biocidal property and moisture absorption, moisture retention, also maintain the original good film property of chitosan, flocculability and biocompatibility and
Degradability, so that it has potential using value in fields such as food industry, medicine, Treatment of Industrial Water, textile processings.
Recently inorganic nano-particle because there is wide spectrum and high-efficiency antimicrobial activity and by extensive concern, such as silver, copper, copper oxide, dioxy
Change titanium, Mg (OH)2And ZnO.ZnO is simple because of preparation, and low cost is more concerned, by as a kind of widely used antibacterial
Agent.In use, metal ion slowly can dissociate out from antibacterial ZnO, and the zinc ion with fungistatic effect is delayed
On The Drug Release, destroys the normal energy metabolism of microorganism, prevents the breeding of pathogen.On the other hand, there is fungistatic effect
Metal ion also can react with the part functional group of protein, nucleic acid, carries out instead even into microbial cell and enzyme
Should, hinder the normal biochemical action of antibacterial and physiological function.Cys is aminoacid common in a kind of organism.Exist
In numerous protein, glutathion, with Ag+, the metal ion such as Hg+, Cu+ can form insoluble mercaptides.I.e. R-
" (M ', M " are respectively 1 valency, divalent metal) to-S-R for S-M ', R-S-M.To sum up, add nano zine oxide, pass through
N-trimethyl chitosan chloride and Cys jointly stabilizing nano zine oxide, reach multiple antibacterial effect.
Thus, invent a kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle herein.This preparation side
Method will have the natural macromolecular n-trimethyl chitosan chloride of antibiotic property, Cys and the nano zine oxide method group by self assembly
Dress up micelle, reach dual antibacterial effect, simple operating steps, practicality and the suitability strong, belong to originality invention.
Summary of the invention
It is an object of the invention to provide a kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle.The party
Method is easy and simple to handle, mild condition, applied widely, i.e. by electrophoretic deposition technique, utilizes n-trimethyl chitosan chloride, L-half Guang ammonia
Acid and nano zine oxide are primitive, prepare hydridization micelle by pH induction self assembly in aqueous phase, then with hydridization micellar solution are
Electrolyte, induces micelle film forming by electrophoretic deposition technique at medical metal surface electricity, obtains based on n-trimethyl chitosan chloride hybridized glue
The nanometer antibacterium coating of bundle.
Another object of the present invention also resides in can be by controlling concentration and the Electrodeposition Conditions of hydridization micellar solution, to nanometer
The performance of antimicrobial coating regulates and controls.
Technical scheme is as follows:
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, its operating procedure is:
(1) preparation of hydridization micellar solution: weigh appropriate n-trimethyl chitosan chloride and be dissolved in the glacial acetic acid aqueous solution of 1% and obtain quaternary ammonium
Change chitosan solution, by formation cysteine solution soluble in water for Cys, by two kinds of solution mixing of preparation, then add
A certain amount of solid nano zinc oxide, continuously stirred, to be mixed uniformly after, regulate the pH value of above-mentioned mixed solution, promote
N-trimethyl chitosan chloride and Cys and nano zine oxide generation self assembly, continue stirring appropriate time, fixing hydridization micelle shape
Looks, obtain hydridization micellar solution；
(2) preparation of nanometer antibacterium coating: ultrasonic cleaning 10～15min in acetone and dehydrated alcohol successively by medical metal,
Room temperature is dried standby, and then with medical metal as negative electrode, platinum plate electrode is anode, the hydridization micellar solution prepared with step (1)
For electrolyte, by electrophoretic deposition technique, prepare nanometer antibacterium coating on medical metal surface.
N-trimethyl chitosan chloride solution concentration prepared in step (1) is 1～5mg/mL, and the concentration of Cys solution is
1～4mg/mL, n-trimethyl chitosan chloride solution and volume ratio 1:1 of Cys solution～1:3, the content 0.8 of nano zine oxide
Mg/mL～3mg/mL, has electrostatic and hydrogen bond action, L-half Guang between n-trimethyl chitosan chloride strand and Cys molecule
It is sulfydryl and metal Zn between propylhomoserin and nano zine oxide2+Between effect.The pH value modification scope of mixed solution is 4～9, continues
Continuous mixing time is 10～30min, and prepared hydridization micelle has pH sensitivity response, ion-sensitive response, micelle chi
Very little between 20～800nm, and micellar surface positively charged.
In step (2), medical metal is selected from titanium or titanium alloy, 316L rustless steel, cobalt-base alloys；The concentration of micelle electrolyte is
3～50mg/mL.The thickness of prepared nanometer antibacterium coating is 10nm～30 μm, and prepared nanometer antibacterium coating has excellent
Different biodegradability, cell compatibility and anti-microbial property.
Beneficial effects of the present invention: novelty of the present invention with n-trimethyl chitosan chloride, Cys and nano zine oxide for primitive,
In aqueous phase, hydridization micelle is prepared in self assembly, induces micelle film forming, preparation to hold concurrently by electrophoretic deposition technique at medical metal surface electricity
Tool biodegradability, cell compatibility and the nano-coating material of anti-microbial property, simple operating steps, material source enriches,
Experimental cost is low, and practicality and the suitability are strong.
Accompanying drawing explanation
Fig. 1 is digital photograph and the micelle TEM shape appearance figure of hydridization micellar solution in embodiment 1；
Fig. 2 is the SEM shape appearance figure of nanometer antibacterium coating in embodiment 2；
Fig. 3 is the fluorescence microscope picture of substrate surface Adherent bacteria in embodiment 3.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the invention is not limited in this.
Embodiment 1
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, concrete preparation process is as follows:
(1) preparation of hydridization micellar solution: n-trimethyl chitosan chloride is dissolved in the glacial acetic acid aqueous solution of 1%, forms 3mg/mL's
N-trimethyl chitosan chloride solution, by the Cys solution of formation 3mg/mL soluble in water for Cys, by two kinds of preparation
Solution equal-volume mixes, and adds certain nano zine oxide so that nano oxidized zinc concentration is 0.8mg/mL, continuously stirred,
To be mixed uniformly after, regulate the pH=6 of above-mentioned mixed solution, promote n-trimethyl chitosan chloride and little molecule L-cysteine and receive
Rice zinc oxide generation self assembly, continues stirring 10min, fixing hydridization micelle pattern, obtains hydridization micellar solution, the number of sample
Under code photo and dry state, shape appearance figure is as shown in Figure 1.
(2) preparation of nanometer antibacterium coating: first by titanium alloy, carries out ultrasonic cleaning with acetone and dehydrated alcohol to it successively
10min, then using above-mentioned pretreated titanium alloy as in the hydridization micellar solution prepared by negative electrode immerses step (1), use
Ability cathode electrophoresis deposition technique, makes the micelle particle of lotus positive electricity to the swimming of medical metal surface and be deposited into micelle film, obtains based on season
The nanometer antibacterium coating of ammonium chitosan hybrid micelle.
Embodiment 2
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, concrete operation step is as follows:
(1) preparation of hydridization micellar solution: n-trimethyl chitosan chloride is dissolved in the glacial acetic acid aqueous solution of 1%, forms 3mg/mL's
N-trimethyl chitosan chloride solution, by the Cys solution of formation 5mg/mL soluble in water for Cys, by two kinds of preparation
Solution 1:2 by volume mixes, and adds certain nano zine oxide so that nano oxidized zinc concentration is 1.0mg/mL, continues
Stirring, to be mixed uniformly after, regulate the pH=7 of above-mentioned mixed solution, promote n-trimethyl chitosan chloride and little molecule L-half Guang ammonia
Acid and nano zine oxide generation self assembly, continue stirring 20min, fixing hydridization micelle pattern, obtain hydridization micellar solution.
(2) preparation of nanometer antibacterium coating: first by cobalt-base alloys, carries out ultrasonic cleaning with acetone and dehydrated alcohol to it successively
10min, more above-mentioned pretreated cobalt-base alloys is got one's things ready micellar solution as the hybridized glue prepared by negative electrode immerses step (1)
In, use ability cathode electrophoresis deposition technique, make the micelle particle of lotus positive electricity to the swimming of medical metal surface and be deposited into micelle film,
To nanometer antibacterium coating based on n-trimethyl chitosan chloride hydridization micelle, the SEM shape appearance figure of coating is as shown in Figure 2.
Embodiment 3
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, concrete operation step is as follows:
(1) preparation of hydridization micellar solution: n-trimethyl chitosan chloride is dissolved in the glacial acetic acid aqueous solution of 1%, forms 5mg/mL's
N-trimethyl chitosan chloride solution, by the Cys solution of formation 3mg/mL soluble in water for Cys, by two kinds of preparation
Solution 1:3 by volume mixes, and adds certain nano zine oxide so that nano oxidized zinc concentration is 3mg/mL, persistently stirs
Mix, to be mixed uniformly after, regulate the pH=8 of above-mentioned mixed solution, promote n-trimethyl chitosan chloride and little molecule L-cysteine
And nano zine oxide generation self assembly, continue stirring 30min, fixing hydridization micelle pattern, obtain hydridization micellar solution.
(2) preparation of nanometer antibacterium coating: first by 316L rustless steel, carries out ultrasonic with acetone and dehydrated alcohol to it successively
Clean 15min, more above-mentioned pretreated 316L rustless steel is molten as the hydridization micelle prepared by negative electrode immerses step (1)
In liquid, use ability cathode electrophoresis deposition technique, make the micelle particle of lotus positive electricity to the swimming of medical metal surface and be deposited into micelle film,
The anti-microbial property such as accompanying drawing 3 obtaining nanometer antibacterium coating based on n-trimethyl chitosan chloride hydridization micelle good shows.
Above-described embodiment is used for illustrating the present invention rather than limiting the invention, and spirit and right in the present invention are wanted
In the protection domain asked, any modifications and changes that the present invention is made, both fall within this bright protection domain.
Claims (5)
1. a nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle, its operating procedure is:
(1) preparation of hydridization micellar solution: weigh appropriate n-trimethyl chitosan chloride and be dissolved in the glacial acetic acid aqueous solution of 1% and obtain quaternary ammonium
Change chitosan solution, by formation cysteine solution soluble in water for Cys, by two kinds of solution mixing of preparation, then add
A certain amount of solid nano zinc oxide, continuously stirred, to be mixed uniformly after, regulate the pH value of above-mentioned mixed solution, promote
N-trimethyl chitosan chloride and Cys and nano zine oxide generation self assembly, continue stirring appropriate time, fixing hydridization micelle shape
Looks, obtain hydridization micellar solution；
(2) preparation of nanometer antibacterium coating: ultrasonic cleaning 10～15min in acetone and dehydrated alcohol successively by medical metal,
Room temperature is dried standby, and then with medical metal as negative electrode, platinum plate electrode is anode, the hydridization micellar solution prepared with step (1)
For electrolyte, by electrophoretic deposition technique, prepare nanometer antibacterium coating on medical metal surface.
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle the most according to claim 1, its
Being characterised by, n-trimethyl chitosan chloride solution concentration prepared in step (1) is 1～5mg/mL, Cys solution dense
Degree is 1～4mg/mL, n-trimethyl chitosan chloride solution and volume ratio 1:1 of Cys solution～1:3, the content of nano zine oxide
0.8mg/mL～3mg/mL, has electrostatic and hydrogen bond action, L-between n-trimethyl chitosan chloride strand and Cys molecule
It is sulfydryl and metal Zn between cysteine and nano zine oxide2+Between effect.
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle the most according to claim 1, its
Being characterised by, in step (1), the pH value modification scope of mixed solution is 4～9, and continuing mixing time is 10～30min, made
Standby hydridization micelle has pH sensitivity response, ion-sensitive response, and micelle size is between 20～800nm, and micelle
Surface positively charged.
The preparation method of a kind of photosensitive n-trimethyl chitosan chloride antimicrobial coating the most according to claim 1, it is characterised in that step
Suddenly in (2), medical metal is selected from titanium or titanium alloy, 316L rustless steel, cobalt-base alloys；The concentration of micelle electrolyte is 3～50mg/mL.
A kind of nanometer antibacterium coating preparation method based on n-trimethyl chitosan chloride hydridization micelle the most according to claim 1, its
Being characterised by, the thickness of nanometer antibacterium coating prepared in step (2) is 10nm～30 μm, and prepared nano-antibacterial is coated with
Layer has biodegradability, cell compatibility and the anti-microbial property of excellence.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108904895A (en) * | 2018-06-20 | 2018-11-30 | 江南大学 | A kind of preparation method of anti-bacterial attachment nano coating |
| CN109276474A (en) * | 2018-09-30 | 2019-01-29 | 江南大学 | A kind of preparation method of nano zine oxide/cationic polysaccharide hybrid nanomaterial |
| CN109364291A (en) * | 2018-10-29 | 2019-02-22 | 西南交通大学 | Flower-shaped coating of organo-mineral complexing and preparation method thereof |
| CN114010837A (en) * | 2021-11-04 | 2022-02-08 | 西安交通大学 | Macromolecular micelle coating for sequentially delivering immunomodulatory factors on nanorod-arrayed surface, and preparation method and application thereof |
| CN114223672A (en) * | 2021-12-31 | 2022-03-25 | 广东粤港澳大湾区国家纳米科技创新研究院 | Composite antibacterial and mildewproof material and application thereof, composite powder coating and preparation method |
| CN114409936A (en) * | 2021-12-29 | 2022-04-29 | 太原理工大学 | Preparation method of composite film added with arginine chitosan and zinc oxide nanoparticles |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108904895A (en) * | 2018-06-20 | 2018-11-30 | 江南大学 | A kind of preparation method of anti-bacterial attachment nano coating |
| CN109276474A (en) * | 2018-09-30 | 2019-01-29 | 江南大学 | A kind of preparation method of nano zine oxide/cationic polysaccharide hybrid nanomaterial |
| CN109276474B (en) * | 2018-09-30 | 2020-11-03 | 江南大学 | Preparation method of nano zinc oxide/cationic polysaccharide hybrid nano particles |
| CN109364291A (en) * | 2018-10-29 | 2019-02-22 | 西南交通大学 | Flower-shaped coating of organo-mineral complexing and preparation method thereof |
| CN109364291B (en) * | 2018-10-29 | 2020-07-31 | 西南交通大学 | Organic-inorganic composite flower-shaped coating and preparation method thereof |
| CN114010837A (en) * | 2021-11-04 | 2022-02-08 | 西安交通大学 | Macromolecular micelle coating for sequentially delivering immunomodulatory factors on nanorod-arrayed surface, and preparation method and application thereof |
| CN114409936A (en) * | 2021-12-29 | 2022-04-29 | 太原理工大学 | Preparation method of composite film added with arginine chitosan and zinc oxide nanoparticles |
| CN114223672A (en) * | 2021-12-31 | 2022-03-25 | 广东粤港澳大湾区国家纳米科技创新研究院 | Composite antibacterial and mildewproof material and application thereof, composite powder coating and preparation method |
| CN114223672B (en) * | 2021-12-31 | 2023-06-13 | 广东粤港澳大湾区国家纳米科技创新研究院 | Composite antibacterial mildew-proof material, application thereof, composite powder coating and preparation method |
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