CN110003499A - A kind of anti-bacterial hydrogel and preparation method thereof - Google Patents
A kind of anti-bacterial hydrogel and preparation method thereof Download PDFInfo
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- CN110003499A CN110003499A CN201910230813.2A CN201910230813A CN110003499A CN 110003499 A CN110003499 A CN 110003499A CN 201910230813 A CN201910230813 A CN 201910230813A CN 110003499 A CN110003499 A CN 110003499A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/02—Polyamines
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- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
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Abstract
The invention discloses a kind of Antimicrobial bacterial cellulose/polyethyleneimine hydrogel preparation methods of novel biocompatibility, belong to biomedical gel technical field, it is characterized in that including the following steps: that bacteria cellulose and polyethyleneimine using epoxychloropropane as crosslinking agent, are prepared bacteria cellulose/polyethyleneimine anti-bacterial hydrogel using the means that in-situ chemical is crosslinked by the preparation (2) of (1) bacteria cellulose (BC) solution.This method has many advantages, such as that plastic is swift in response, reaction system is simple and gel plasticity is high.Due to the presence of bacteria cellulose, the high mechanical strength of anti-bacterial hydrogel prepared by the present invention.Compared with traditional small molecule anti-biotic material, bacteria cellulose prepared by the present invention/polyethyleneimine anti-bacterial hydrogel has the fungistatic effect of wide spectrum and biocompatibility is good.
Description
Technical field
The present invention relates to biomedical gel technical field, in particular to the antibacterial bacterial fibers of a kind of biocompatibility
Element/polyethyleneimine hydrogel fast preparation method.
Background technique
Nowadays, although the mankind have made significant headway in medical treatment & health field, by virus, bacterium and fungi etc.
Infectious disease caused by pathogen is still a kind of main health threat, and can be converted into extensive socioeconomic problem.
And with the development of the social economy, people also constantly promote the pursuit of quality of life and healthy quality, antimicrobial product is by people
Be considered have one of new type health product with broad prospects for development.Traditional anti-biotic material is by chemistry or physics
Method is on the surface of the material or ontology introduces some antibacterial agents (such as antibiotic, quaternary ammonium salt and fungicide) to assign these biologies doctor
With the certain antibacterial ability of material.But since the small molecule antibacterial agent of antibiotics usually has specificity and is easy to cause
It is bacterial resistance occurred.Therefore, developing the novel anti-biotic material with broad spectrum antibacterial ability just seems extremely urgent.
Hydrogel is that have the new of three-dimensional (3D) reticular structure by what is be physically or chemically cross-linked to form by hydrophilic polymer
Type polymer-function material can retain a large amount of water in polymer network.Since hydrogel has excellent bio-compatible
Property, it is therefore widely used in the various biomedical materials fields such as drug conveying, organizational project, wound healing and antibacterial.
Anti-bacterial hydrogel not only has the characteristic of multiple polymers, good compatibility, and can effectively resist bacterium infection, suppression
The generation of bacterial drug resistance processed promotes wound healing.Therefore, in recent years, anti-bacterial hydrogel becomes a kind of novel wound dressing
Applied to medical field.
Biopolymer is attract attention in hydrogel production, it is a kind of with biocompatibility and ecology
Environmental-friendly renewable resource.Bacteria cellulose (BC) is one kind by bacteriogenic natural biological copolymer.BC has one
A little unique properties, such as bioactivity, biodegradability, biocompatibility, nontoxic, tough without allergic reaction, good machinery
Property, excellent water-retaining property, higher purity, higher porosity and higher crystallinity etc., make it bio-medical water-setting
The important raw material of glue.Pain can be effectively relieved in bacteria cellulose based aquagel, there is good adhesion, it effectively prevent thin
The invasion of bacterium is infected, and is conducive to skin histology growth, is promoted the quick healing of wound, is had for moisture and electrolyte good logical
Permeability.
Polyethyleneimine (PEI) is a kind of water-soluble polymer generated by the polymerization of aziridine.It is not
Complete linear polymer, but a kind of includes primary amine, the part branched polymer of secondary amine and tertiary amine.PEI has excellent suppression
Bacterium performance.Using epoxychloropropane as crosslinking agent, bacteria cellulose and polyethyleneimine are used to the means system of in-situ chemical crosslinking
Detailed fungin/polyethyleneimine anti-bacterial hydrogel.The advantages of obtained hydrogel has had both two kinds of polymer has excellent
Biocompatibility, mechanical tenacity and bacteriostasis property, biomedical materials field can be widely used in.
There are some problems: traditional anti-biotic material, such as quaternary ammonium salt for the anti-bacterial hydrogel of existing literature report
(CN105999406A), antibiotic etc. is easy to cause bacterial resistance occurred, and the antibacterial agents such as nano silver (CN1291667A) are deposited
In the enrichment problem of antibacterial agent；Select polypeptide (CN201310520058), albumen (CN201710130499) etc. as plastic at
Point, price is more expensive.
Summary of the invention
The purpose of the present invention is to provide a kind of Antimicrobial bacterial cellulose/polyethyleneimine aqueous amines of novel biocompatibility
Gel and its method quickly prepared.The hydrogel has excellent antibacterial activity, and antibacterial activity is lasting.
Technical principle of the invention:
It is with the good bacteria cellulose biopolymer of biocompatibility and polyethyleneimine macromolecule polymer material
Main material prepares bacteria cellulose/polyethyleneimine using the means that in-situ chemical is crosslinked using epoxychloropropane as crosslinking agent
Anti-bacterial hydrogel.
To achieve the goals above, above-mentioned technical problem, the technical solution adopted by the present invention are solved are as follows:
(1) preparation of bacterial cellulose solution
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, BC solution is prepared.
(2) bacteria cellulose/polyethyleneimine hydrogel preparation
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution of 2ml various concentration is added in mixture simultaneously rapidly
Stirring is to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, then use
Deionized water cleaning, removes unreacted substance and various foreign ions, stores for future use at room temperature later.
Moreover, the concentration of the bacterial cellulose suspension is 2wt/v%.
Moreover, average fiber length is 10-100 microns in the bacterial cellulose suspension.
Moreover, the molecular weight of the polyethyleneimine is 1800.
Moreover, the concentration of the polyethylenimine solution is respectively 0wt, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%
And 10wt%.
Moreover, concentration of the crosslinking agent epoxychloropropane in bacteria cellulose/polyethyleneimine mixture solution is
3.2v/v%.
Beneficial effects of the present invention:
(1) present invention is using epoxychloropropane as crosslinking agent, prepares bacteria cellulose/poly- using the means that in-situ chemical is crosslinked
Aziridine anti-bacterial hydrogel has many advantages, such as that reaction system is simple, plastic is swift in response and gel plasticity is high.
(2) bacteria cellulose prepared by the present invention/polyethyleneimine anti-bacterial hydrogel is to Escherichia coli and golden yellow grape
Coccus all has good fungistatic effect.
(3) compared with traditional small molecule anti-biotic material, the present invention provides a kind of broader spectrum of antimicrobial composite materials
Preparation method.
(4) anti-bacterial hydrogel prepared by the present invention has good biocompatibility, and biodegradability is nontoxic, and machine
Tool intensity is high.
(5) anti-bacterial hydrogel plasticity prepared by the present invention is high, and toughness is high, can be according to actual need
It wants, is designed to different shapes.
Detailed description of the invention
Fig. 1 is bacteria cellulose prepared by the present invention/polyethyleneimine anti-bacterial hydrogel effect picture.
Fig. 2 is bacteria cellulose of the present invention/polyethyleneimine anti-bacterial hydrogel to Escherichia coli and staphylococcus aureus
Bactericidal test effect picture.(A, B are the Bactericidal test effect picture of hydrogel Escherichia coli；C, D is hydrogel to golden yellow
Staphylococcic Bactericidal test effect picture；BCP0, BCP1, BCP2, BCP3, BCP4, BCP5, and BCP6 respectively represent addition
Preparation-obtained gel when the concentration of PEI is respectively 0wt, 1wt%, 2wt%, 3wt%, 4wt%, 5wt% and 10wt%.)
Fig. 3 be rheometer of the present invention measure bacteria cellulose/polyethyleneimine anti-bacterial hydrogel storage modulus (G ') and
Loss modulus (G ") with frequency change curve.(A, B, C, D, E, F and G respectively represent gel BCP0, BCP1, BCP2,
The storage modulus (G ') and loss modulus (G ") of BCP3, BCP4, BCP5, and BCP6 with frequency change curve.)
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
The every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
A kind of preparation method of Antimicrobial bacterial cellulose/polyethyleneimine hydrogel, steps are as follows:
(1) bacteria cellulose film is crushed using mechanical homogenisation method, obtains bacterial fibers by the preparation of bacterial cellulose solution
Element homogenate.Homogenate high speed centrifugation 10 minutes will obtained later, to remove extra moisture, then with 12% urea and 7%
NaOH aqueous dissolution by bacteria cellulose be homogenized dissolve, stir evenly, bacterial cellulose solution is prepared.
(2) bacteria cellulose/polyethyleneimine hydrogel preparation, at room temperature, by a certain amount of epoxychloropropane solution
It is added in 4ml bacterial cellulose solution.60min is stirred at room temperature to obtain a uniform viscosity solution.Then, not by 2ml
PEI solution with concentration is added in mixture and is stirred rapidly to obtain uniform mixture solution.Gel will be in a few houres
Within quickly formed, after obtained gel is placed for 24 hours, with 70% ethanol washing several times, if then being cleaned with deionized water
Dry time, room temperature storage is spare.
Embodiment 1
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, the BC solution of 2% (dry weight wt/v%) is prepared.
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution that 2ml concentration is 1wt% is added in mixture simultaneously
Stirring is rapidly to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, so
It is cleaned afterwards with deionized water, removes unreacted substance and various foreign ions, store for future use at room temperature later.
Embodiment 2
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, the BC solution of 2% (dry weight wt/v%) is prepared.
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution that 2ml concentration is 2wt% is added in mixture simultaneously
Stirring is rapidly to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, so
It is cleaned afterwards with deionized water, removes unreacted substance and various foreign ions, store for future use at room temperature later.
Embodiment 3
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, the BC solution of 2% (dry weight wt/v%) is prepared.
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution that 2ml concentration is 3wt% is added in mixture simultaneously
Stirring is rapidly to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, so
It is cleaned afterwards with deionized water, removes unreacted substance and various foreign ions, store for future use at room temperature later.
Embodiment 4
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, the BC solution of 2% (dry weight wt/v%) is prepared.
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution that 2ml concentration is 5wt% is added in mixture simultaneously
Stirring is rapidly to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, so
It is cleaned afterwards with deionized water, removes unreacted substance and various foreign ions, store for future use at room temperature later.
Embodiment 5
Bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, obtains bacteria cellulose homogenate.It obtains
Homogenate be centrifuged 10 minutes with the revolving speed of 10,000rpm/min, to remove extra moisture, be then dissolved in the urea containing 12%
It in the aqueous solution of 7% NaOH, stirs evenly, the BC solution of 2% (dry weight wt/v%) is prepared.
At room temperature, a certain amount of epoxychloropropane solution is added in 4ml bacterial cellulose solution.It is stirred at room temperature
60min is to obtain a uniform viscosity solution.Then, the PEI solution that 2ml concentration is 10wt% is added in mixture simultaneously
Stirring is rapidly to obtain uniform mixture solution.After obtained gel is placed for 24 hours, with 70% ethanol washing several times, so
It is cleaned afterwards with deionized water, removes unreacted substance and various foreign ions, store for future use at room temperature later.
Claims (6)
1. a kind of Antimicrobial bacterial cellulose/polyethyleneimine hydrogel and preparation method thereof, which is characterized in that including following step
It is rapid:
(1) preparation of bacterial cellulose solution: bacteria cellulose film is crushed by mechanical homogenisation method using tissue refiner, is obtained
Bacteria cellulose homogenate.Obtained homogenate was with revolving speed centrifugation 10 minutes of 10,000rpm/min, to remove extra moisture, so
It is dissolved in the aqueous solution containing 12% urea and 7% NaOH, stirs evenly, bacterial cellulose solution is prepared afterwards.
(2) bacteria cellulose/polyethyleneimine hydrogel preparation: at room temperature, a certain amount of epoxychloropropane solution is added
Into 4ml bacterial cellulose solution.60min is stirred at room temperature to obtain a uniform viscosity solution.Then, 2ml difference is dense
The PEI solution of degree is added in mixture and is stirred rapidly to obtain uniform mixture solution.Obtained gel is placed for 24 hours
Afterwards, with 70% ethanol washing several times, then cleaned with deionized water, remove unreacted substance and various foreign ions,
It stores for future use at room temperature later.
2. the preparation method of bacterial cellulose solution according to claim 1, it is characterised in that: the bacteria cellulose suspends
The concentration of liquid is 2wt/v%.
3. the preparation method of bacterial cellulose solution according to claim 1, it is characterised in that: the bacteria cellulose suspends
Average fiber length is 10-100 microns in liquid.
4. bacteria cellulose/polyethyleneimine hydrogel preparation method according to claim 1, it is characterised in that: described
The molecular weight of polyethyleneimine is 1800.
5. bacteria cellulose/polyethyleneimine hydrogel preparation method according to claim 1, it is characterised in that: described
The concentration of polyethylenimine solution is respectively 0wt, 1wt%, 2wt%, 3wt%, 4wt%, 5wt% and 10wt%.
6. bacteria cellulose/polyethyleneimine hydrogel preparation method according to claim 1, it is characterised in that: described
Concentration of the crosslinking agent epoxychloropropane in bacteria cellulose/polyethyleneimine mixture solution is 3.2v/v%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110804192A (en) * | 2019-09-29 | 2020-02-18 | 天津科技大学 | Cellulose antibacterial hydrogel and preparation method thereof |
| CN111303449A (en) * | 2020-01-17 | 2020-06-19 | 华中科技大学 | Degradable electroactive bacterial cellulose/MXene composite hydrogel and preparation and application thereof |
| CN112341832A (en) * | 2020-11-25 | 2021-02-09 | 董思民 | Freeze-thaw abrasion resistant pavement repair material and production process and application thereof |
| CN112724422A (en) * | 2020-12-29 | 2021-04-30 | 兰州大学 | Bacteriostatic wheat straw cellulose composite hydrogel and preparation method and application thereof |
| CN114766477A (en) * | 2022-05-10 | 2022-07-22 | 浙江大学 | Application of polyethyleneimine-cellulose composite gel |
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| CN106519285A (en) * | 2016-09-23 | 2017-03-22 | 嘉兴赛维环保科技有限公司 | Preparation method for three-dimensional network structure flocculation material structured by bacterial cellulose |
| CN108187119A (en) * | 2018-01-16 | 2018-06-22 | 浙江理工大学 | A kind of antibacterial anti hemorrhagic material based on cellulose and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110804192A (en) * | 2019-09-29 | 2020-02-18 | 天津科技大学 | Cellulose antibacterial hydrogel and preparation method thereof |
| US20210015966A1 (en) * | 2019-09-29 | 2021-01-21 | Tianjin University Of Science And Technology | Antibacterial Cellulose Hydrogels and Preparation Method therefor |
| CN111303449A (en) * | 2020-01-17 | 2020-06-19 | 华中科技大学 | Degradable electroactive bacterial cellulose/MXene composite hydrogel and preparation and application thereof |
| CN112341832A (en) * | 2020-11-25 | 2021-02-09 | 董思民 | Freeze-thaw abrasion resistant pavement repair material and production process and application thereof |
| CN112341832B (en) * | 2020-11-25 | 2022-05-27 | 河南省第一公路工程有限公司 | Freeze-thaw abrasion resistant pavement repair material and production process and application thereof |
| CN112724422A (en) * | 2020-12-29 | 2021-04-30 | 兰州大学 | Bacteriostatic wheat straw cellulose composite hydrogel and preparation method and application thereof |
| CN114766477A (en) * | 2022-05-10 | 2022-07-22 | 浙江大学 | Application of polyethyleneimine-cellulose composite gel |
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