CN109749137A - A kind of preparation method of aquagel dressing - Google Patents
A kind of preparation method of aquagel dressing Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of aquagel dressing.Absorbent cotton is hydrolyzed using the concentrated sulfuric acid, prepares Cellulose nanocrystal body；Using sodium periodate oxidation Cellulose nanocrystal body, dialdehyde Cellulose nanocrystal body is prepared；Dialdehyde Cellulose nanocrystal body is grafted using polymerizable cationic monomer, prepares modified cellulose nanocrystal；Chitosan-acetic acid solution and modified cellulose nanocrystal suspension are mixed to get composite hydrogel；Freeze-drying hydrogel obtains modified cellulose nanocrystal/chitosan composite hydrogel dressing.Entire production process cleaning, environmental pollution is small and low energy consumption；Prepared modified nanometer cellulose crystal/chitosan composite hydrogel dressing good biocompatibility, totally biodegradable, water retention with higher and mechanical strength, while also there is good antibiotic property.
Description
Technical field
The present invention relates to technical field of biological materials, more particularly to a kind of preparation method of aquagel dressing.
Background technique
Ideal dressing should be able to maintain one wet environment of wound or the surface of a wound, have good gas permeability, can
Promote cell Proliferation, the exudate of wound or the surface of a wound can be discharged as the barrier for stopping microorganism but also rapidly, while should
Nontoxic, no antigen is not likely to produce tissue adhesion.Compared to traditional wound or Wound dressing, such as gauze, cotton pad, wool, each
Class oil gauze etc., aerogel dressing can provide preferably ventilative, moisture-inhibiting, barrier bacterium invades and controls and absorb diffusate etc.
Characteristic, so that wound or the surface of a wound are in good cell growth healing environment.In addition, aerogel dressing can adhere well to wound or
At the surface of a wound, and glutinous wound will not be stained in more change dressings or the surface of a wound causes secondary injury, therefore aerogel dressing is widely answered
For in medical field.Chitosan is from a wealth of sources, cheap and easy to get, bio-compatible, biodegradable, natural antibacterial, is to prepare water
The ideal material of gel dressing.Aquagel dressing should meet the following conditions: (1) can absorb wound or the surface of a wound rapidly
Diffusate, and keep the wet of the surface of a wound；(2) it breathes freely；(3) antibacterial；(4) mechanical strength；(5) with the bonding of the surface of a wound.In order into one
Walk the water conservation for improving aquagel dressing, ventilative, mechanical strength and antibiotic property, the present invention is with Cellulose nanocrystal body
Basis prepares modified cellulose nanocrystal by sodium periodate oxidation and further graft polymerization.Modified cellulose nanometer
Plane of crystal not only contains aldehyde radical, but also contains cation graft chain.Modified cellulose nanocrystal and chitosan-acetic acid solution
Blending can prepare composite hydrogel, and wherein modified cellulose nanocrystal plays the effect of enhancing and crosslinking simultaneously, and preparation is answered
Heshui gel water retention with higher, excellent gas permeability and mechanical strength, while also there is good antibiotic property.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of preparation methods of aquagel dressing, can prepare
The modified nanometer cellulose crystal of good biocompatibility/chitosan composite hydrogel dressing, dressing water retention with higher
And mechanical strength, while also there is good antibiotic property.
In order to solve the above technical problems, one technical scheme adopted by the invention is that:
A kind of preparation method of aquagel dressing is provided, the specific steps of which are as follows:
(1) absorbent cotton of 1 mass fraction is added in the concentrated sulfuric acid of 10~30 mass fractions, the mechanical stirring at 40~60 DEG C
Reaction 0.5~2 hour, it is 7 that sodium hydroxide, which is added, and adjusts the pH of feed liquid, then carries out high speed centrifugation several times, it is white to collect upper layer
Color suspension obtains Cellulose nanocrystal liquid suspension after dialysis；
(2) sodium metaperiodate of 1 mass fraction Cellulose nanocrystal liquid suspension and 1 ~ 7 mass fraction prepared by step (1) is taken
Mixing, 40~60 DEG C, be protected from light under the conditions of react 2~8 hours, the ethylene glycol of 1~7 mass fraction is added, and the reaction was continued 0.5~1
Hour, dialdehyde Cellulose nanocrystal liquid suspension is obtained after dialysis；
(3) 1 mass fraction dialdehyde Cellulose nanocrystal liquid suspension prepared by step (2) and 1~4 mass fraction cation are taken
Monomer mixing, is added 0.2~0.4 mass fraction initiator under 40~60 DEG C, nitrogen protection, reacts 3~5 hours, after dialysis
Obtain modified nanometer cellulose Crystal suspensions；
(4) it takes the chitosan of 1 mass fraction to be dissolved in the acetum of 50~100 mass fractions 1~2%, is added 0.1~0.2
The glycerol of mass fraction is sufficiently mixed, and takes 20~50 mass fractions modified nanometer cellulose crystal suspension prepared by step (3)
Liquid is mixed with 50~100 mass fraction chitosan-acetic acid solutions, and ultrasound 20~60 minutes at a temperature of 25~50 DEG C stand and formed
Modified cellulose nanocrystal/chitosan composite hydrogel, obtains hydrogel lyophilized products after freeze-drying.
In a preferred embodiment of the present invention, in step (3), the cationic monomer is acrylyl oxy-ethyl front three
Ammonium chloride or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride.
In a preferred embodiment of the present invention, in step (3), the initiator is ammonium ceric nitrate and potassium peroxydisulfate
The mixing mass ratio of mixture, ammonium ceric nitrate and potassium peroxydisulfate is 1:1 ~ 1:5.
In a preferred embodiment of the present invention, in step (4), the molecular weight of the chitosan is 10~2,000,000.
The present invention also provides a kind of modified nanometer cellulose crystal prepared using the above method.
The present invention also provides a kind of modified cellulose nanocrystal/chitosan compound water congealings prepared using the above method
Glue.
The beneficial effects of the present invention are: a kind of preparation method of aquagel of the present invention, is hydrolyzed de- using the concentrated sulfuric acid
Rouge cotton prepares Cellulose nanocrystal body using sodium periodate oxidation Cellulose nanocrystal body and prepares dialdehyde Cellulose nanocrystal
Body is grafted dialdehyde Cellulose nanocrystal body using polymerizable cationic monomer, modified cellulose nanocrystal is prepared, by chitosan
Acetum and modified cellulose nanocrystal suspension are mixed to get composite hydrogel；Freeze-drying hydrogel is modified
Cellulose nanocrystal body/chitosan composite hydrogel dressing.Modified nanometer cellulose crystal/chitosan composite hydrogel dressing is raw
Object compatibility is good, totally biodegradable, water retention with higher and mechanical strength, while also having good antibiotic property.
Detailed description of the invention
Fig. 1 is the chemical structural formula of modified cellulose nanocrystal in the present invention；
Fig. 2 is modified cellulose nanocrystal/chitosan composite hydrogel dressing scanning electron microscope (SEM) photo.
Specific embodiment
The preferred embodiments of the present invention will be described in detail with reference to the accompanying drawing, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art, so as to make a clearer definition of the protection scope of the present invention.
Preparation step in the present invention specifically divides four steps:
(1) concentrated sulfuric acid hydrolysis absorbent cotton prepares Cellulose nanocrystal body；
(2) sodium periodate oxidation Cellulose nanocrystal body prepares dialdehyde Cellulose nanocrystal body；
(3) graft polymerization of the cationic monomer in dialdehyde Cellulose nanocrystal body surface face prepares modified cellulose nanocrystal；
(4) modified cellulose nanocrystal/chitosan composite hydrogel dressing preparation.
The nanocrystal of modified cellulose prepared by the present invention/chitosan composite hydrogel properties can be used following
Index is detected:
(1) pattern: aerogel dressing is through liquid nitrogen brittle failure, section metal spraying, using the SU-1510 type scanning electron of Hitachi, Japan
Microscope observes its cross-sectional morphology under 5 kV high pressures.
(2) swelling behavior (water retention): by aerogel dressing, drying to constant weight.Weigh Wd(g) it immerses in deionized water afterwards
Enough for a long time, it takes out and blots its surface moisture with filter paper, weigh Ws(g immediately).The Equilibrium swelling ratio (Q, %) of sample is counted
Calculate formula are as follows:
(3) porosity (gas permeability): the porosity test of aerogel dressing uses ethyl alcohol method of substitution, and specific practice is to use first
It is respectively a(mm that micrometer caliper, which measures a fritter aerogel dressing sample length), b(mm), c(mm), weight Ws(g)；
Be d(g/cm3 by density) dehydrated alcohol be packed into container (volume account for about container 1/2), then by weight be Ws(g) compound water congealing
Glue dressing merging is equipped in the container of ethyl alcohol and is weighed as W1(g), make ethyl alcohol full of in the hole of sample after vacuum outgas, takes
Weigh after sample W2(g out)；Porosity (P, %) formula is as follows:
。
Embodiment 1
(1) 1 part of (following number is all mass fraction) absorbent cotton is added in 20 part 64% of the concentrated sulfuric acid, is 45 DEG C in temperature,
It is reacted under 400r/min~600r/min mechanical agitation 1 hour, high speed centrifugation, collects upper layer white suspension after reaction
Liquid, and adding alkali to adjust pH is weakly acidic pH, dialysis obtains Cellulose nanocrystal liquid suspension；
(2) 3 parts of sodium metaperiodates are added in the Cellulose nanocrystal liquid suspension of 50 parts of steps (1) preparation, are 45 DEG C in temperature
Be protected from light under the conditions of react 5 hours；3 parts of glycol reactions are added 1 hour and dialyse 3 days, obtains dialdehyde Cellulose nanocrystal body
Suspension；
(3) 2 parts of acrylyl oxy-ethyl-trimethyl salmiacs are added to the dialdehyde Cellulose nanocrystal body of 100 parts of steps (2) preparation
In suspension, in acid condition, 0.05 part of ammonium ceric nitrate and 0.05 part of potassium peroxydisulfate is added, is 50 DEG C in temperature, nitrogen ring
It is reacted 4 hours under border, dialysis obtains modified cellulose nanocrystal suspension；
(4) chitosan that 1 part of molecular weight is 1,000,000 at room temperature is dissolved in 50 part 1.5% of acetum, and 0.1 part of addition is sweet
Oil, which is sufficiently mixed, is configured to chitosan-acetic acid solution, and the modified cellulose nanocrystal suspension of 20 parts of steps (3) preparation is added,
45 DEG C ultrasound 30 minutes, vacuum decompression deaeration is placed at room temperature for 24 hours to form hydrogel, obtains modified cellulose after freeze-drying
Nanocrystal/chitosan composite hydrogel dressing.
Embodiment 2
(1) 1 part of absorbent cotton is added in 20 part 64% of the concentrated sulfuric acid, is 45 DEG C in temperature, anti-under 600r/min mechanical agitation
It answers 1 hour, after reaction high speed centrifugation, collect upper layer white suspension and the sodium hydroxide of 0.1N is added to adjust pH be in close
Property, dialysis obtains Cellulose nanocrystal liquid suspension in 3 days；
(2) 3 parts of sodium metaperiodates are added in the Cellulose nanocrystal liquid suspension of 50 parts of steps (1) preparation, are 45 DEG C in temperature
Be protected from light under the conditions of react 5 hours；3 parts of glycol reactions are added 1 hour and dialyse 3 days, obtains dialdehyde Cellulose nanocrystal body
Suspension；
(3) 2 parts of acrylyl oxy-ethyl-trimethyl salmiacs are added to the dialdehyde Cellulose nanocrystal body of 100 parts of steps (2) preparation
In suspension, in acid condition, 0.05 part of ammonium ceric nitrate and 0.05 part of potassium peroxydisulfate is added, is 50 DEG C in temperature, nitrogen ring
It is reacted 4 hours under border, dialysis obtains modified cellulose nanocrystal suspension in 3 days；
(4) chitosan that 1 part of molecular weight is 1,000,000 at room temperature is dissolved in 50 part 1.5% of acetum, and 0.1 part of addition is sweet
Oil, which is sufficiently mixed, is configured to chitosan-acetic acid solution, and the modified cellulose nanocrystal suspension of 30 parts of steps (3) preparation is added,
45 DEG C ultrasound 30 minutes, vacuum decompression deaeration is placed at room temperature for 24 hours to form hydrogel, obtains modified cellulose after freeze-drying
Nanocrystal/chitosan composite hydrogel dressing.
Embodiment 3
(1) 1 part of absorbent cotton is added in 20 part 64% of the concentrated sulfuric acid, is 45 DEG C in temperature, anti-under 600r/min mechanical agitation
It answers 1 hour, after reaction high speed centrifugation, collect upper layer white suspension and the sodium hydroxide of 0.1N is added to adjust pH be in close
Property, dialysis obtains Cellulose nanocrystal liquid suspension in 3 days；
(2) 3 parts of sodium metaperiodates are added in the Cellulose nanocrystal liquid suspension of 50 parts of steps (1) preparation, are 45 DEG C in temperature
Be protected from light under the conditions of react 5 hours；3 parts of glycol reactions are added 1 hour and dialyse 3 days, obtains dialdehyde Cellulose nanocrystal body
Suspension；
(3) 2 parts of acrylyl oxy-ethyl-trimethyl salmiacs are added to the dialdehyde Cellulose nanocrystal body of 100 parts of steps (2) preparation
In suspension, in acid condition, 0.05 part of ammonium ceric nitrate and 0.05 part of potassium peroxydisulfate is added, is 50 DEG C in temperature, nitrogen ring
It is reacted 4 hours under border, dialysis obtains modified cellulose nanocrystal suspension in 3 days；
(4) chitosan that 1 part of molecular weight is 1,000,000 at room temperature is dissolved in 50 part 1.5% of acetum, and 0.1 part of addition is sweet
Oil, which is sufficiently mixed, is configured to chitosan-acetic acid solution, and the modified cellulose nanocrystal suspension of 40 parts of steps (3) preparation is added,
45 DEG C ultrasound 30 minutes, vacuum decompression deaeration is placed at room temperature for 24 hours to form hydrogel, obtains modified cellulose after freeze-drying
Nanocrystal/chitosan composite hydrogel dressing.
Embodiment 4
(1) 1 part of absorbent cotton is added in 20 part 64% of the concentrated sulfuric acid, is 45 DEG C in temperature, anti-under 600r/min mechanical agitation
It answers 1 hour, after reaction high speed centrifugation, collect upper layer white suspension and the sodium hydroxide of 0.1N is added to adjust pH be in close
Property, dialysis obtains Cellulose nanocrystal liquid suspension in 3 days；
(2) 3 parts of sodium metaperiodates are added in the Cellulose nanocrystal liquid suspension of 50 parts of steps (1) preparation, are 45 DEG C in temperature
Be protected from light under the conditions of react 5 hours；3 parts of glycol reactions are added 1 hour and dialyse 3 days, obtains dialdehyde Cellulose nanocrystal body
Suspension；
(3) 2 parts of acrylyl oxy-ethyl-trimethyl salmiacs are added to the dialdehyde Cellulose nanocrystal body of 100 parts of steps (2) preparation
In suspension, in acid condition, 0.05 part of ammonium ceric nitrate and 0.05 part of potassium peroxydisulfate is added, is 50 DEG C in temperature, nitrogen ring
It is reacted 4 hours under border, dialysis obtains modified cellulose nanocrystal suspension in 3 days；
(4) chitosan that 1 part of molecular weight is 1,000,000 at room temperature is dissolved in 50 part 1.5% of acetum, and 0.1 part of addition is sweet
Oil, which is sufficiently mixed, is configured to chitosan-acetic acid solution, and the modified cellulose nanocrystal suspension of 50 parts of steps (3) preparation is added,
45 DEG C ultrasound 30 minutes, vacuum decompression deaeration is placed at room temperature for 24 hours to form hydrogel, obtains modified cellulose after freeze-drying
Nanocrystal/chitosan composite hydrogel dressing.
A kind of water balance swelling of modified cellulose nanocrystal/chitosan composite hydrogel dressing prepared by the present invention
It spends as shown in table 1 with porosity:
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to be said using the present invention
Equivalent structure or equivalent flow shift made by bright book and accompanying drawing content is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of aquagel dressing, which is characterized in that the specific steps of which are as follows:
(1) absorbent cotton of 1 mass fraction is added in the concentrated sulfuric acid of 10~30 mass fractions, the mechanical stirring at 40~60 DEG C
Reaction 0.5~2 hour, it is 7 that sodium hydroxide, which is added, and adjusts the pH of feed liquid, then carries out high speed centrifugation several times, it is white to collect upper layer
Color suspension obtains Cellulose nanocrystal liquid suspension after dialysis；
(2) sodium metaperiodate of 1 mass fraction Cellulose nanocrystal liquid suspension and 1 ~ 7 mass fraction prepared by step (1) is taken
Mixing, 40~60 DEG C, be protected from light under the conditions of react 2~8 hours, the ethylene glycol of 1~7 mass fraction is added, and the reaction was continued 0.5~1
Hour, dialdehyde Cellulose nanocrystal liquid suspension is obtained after dialysis；
(3) 1 mass fraction dialdehyde Cellulose nanocrystal liquid suspension prepared by step (2) and 1~4 mass fraction cation are taken
Monomer mixing, is added 0.2~0.4 mass fraction initiator under 40~60 DEG C, nitrogen protection, reacts 3~5 hours, after dialysis
Obtain modified nanometer cellulose Crystal suspensions；
(4) it takes the chitosan of 1 mass fraction to be dissolved in the acetum of 50~100 mass fractions 1~2%, is added 0.1~0.2
The glycerol of mass fraction is sufficiently mixed, and takes 20~50 mass fractions modified nanometer cellulose crystal suspension prepared by step (3)
Liquid is mixed with 50~100 mass fraction chitosan-acetic acid solutions, and ultrasound 20~60 minutes at a temperature of 25~50 DEG C stand and formed
Modified cellulose nanocrystal/chitosan composite hydrogel, obtains hydrogel lyophilized products after freeze-drying.
2. the preparation method of aquagel dressing according to claim 1, which is characterized in that in step (3), institute
Stating cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride.
3. the preparation method of aquagel dressing according to claim 1, which is characterized in that in step (3), institute
Initiator is stated as the mixture of ammonium ceric nitrate and potassium peroxydisulfate, the mixing mass ratio of ammonium ceric nitrate and potassium peroxydisulfate is 1:1 ~ 1:5.
4. the preparation method of aquagel dressing according to claim 1, which is characterized in that described in step (4)
The molecular weight of chitosan is 10~2,000,000.
5. the modified nanometer cellulose crystal of the method preparation according to claim 1 ~ one of 4.
6. modified cellulose nanocrystal/chitosan composite hydrogel of the method preparation according to claim 1 ~ one of 4.
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| CN110947022A (en) * | 2019-08-01 | 2020-04-03 | 安徽省小山卫生材料有限公司 | Preparation method of chitosan-based composite antibacterial dressing |
| CN111155216A (en) * | 2020-02-13 | 2020-05-15 | 深圳市亚骏宇科技有限公司 | Antibacterial fiber composition and fabric and application thereof |
| CN113797386A (en) * | 2021-09-13 | 2021-12-17 | 浙江大学 | Conductive hydrogel/reactive oxygen species response polyurethane composite membrane loaded with doxycycline hydrochloride and preparation method thereof |
| CN117679555A (en) * | 2024-02-04 | 2024-03-12 | 吉林农业科技学院 | Larch cellulose hydrogel, preparation method thereof and application of larch cellulose hydrogel in promoting bone repair |
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| CN117679555A (en) * | 2024-02-04 | 2024-03-12 | 吉林农业科技学院 | Larch cellulose hydrogel, preparation method thereof and application of larch cellulose hydrogel in promoting bone repair |
| CN117679555B (en) * | 2024-02-04 | 2024-04-12 | 吉林农业科技学院 | Larch cellulose hydrogel, preparation method thereof and application of larch cellulose hydrogel in promoting bone repair |
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Application publication date: 20190514 |