CN107929794A - A kind of cellulose chitosan combine dressing based on chemical crosslinking and preparation method thereof - Google Patents
A kind of cellulose chitosan combine dressing based on chemical crosslinking 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
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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
- A61L15/42—Use of materials characterised by their function or physical properties
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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
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/425—Porous materials, e.g. foams or sponges
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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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
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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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
- A61L2300/418—Agents promoting blood coagulation, blood-clotting agents, embolising agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/80—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special chemical form
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The present invention relates to a kind of cellulose chitosan combine dressing based on chemical crosslinking and preparation method thereof, the combine dressing includes epoxy silane coupling agent, cellulose and chitosan or chitosan derivatives, with even porous net structure, chitosan or chitosan derivatives are crosslinked the surface for being evenly coated at cellulose skeleton by epoxy silane coupling agent;Preparation method includes:Suspension mixed synthesis, the synthesis of the cellulose chitosan combine dressing based on chemical crosslinking.The method of the present invention is simple, and easily operated, cost is low, environmental protection;The cellulose chitosan combine dressing based on chemical crosslinking that the present invention obtains has good mechanicalness and pliability, liquid absorption amount is big and good permeability, the material, which is avoided, causes damage the Skin Cell of wound using the dissolution of process small molecular, it can promote blood coagulation and avoid wound infection, have wide practical use in medical dressing field.
Description
Technical field
The invention belongs to medical dressing and its preparation field, more particularly to a kind of cellulose-shell based on chemical crosslinking gathers
Sugared combine dressing and preparation method thereof.
Background technology
Organ of the skin as human body maximum, is to protect in-vivo tissue and organ from external environmental interference and stimulation, dimension
Hold the important barrier of inside of human body environmental balance.If skin is damaged, healing in time, can not cause wound inflammation or other
Pathological change.Medical dressing one kind can effectively protect wound, promote the material of wound healing.Preferable medical dressing should
With control wound fluid, wound infection is avoided, wound moist environment is kept and promotes wound healing and other effects.
Cellulose is the natural polymer that reserves are most abundant in nature, because it is with good biocompatibility, biology
Degradability, the application in technical field of biological material especially dressing field are more and more wider.But simple cellulosic material does not possess
Avoid wound infection, promote the effect of wound healing.Chitosan is through deacetylated by the chitin being widespread in nature
Effect obtains, not only bio-compatible, biodegradable, while has other performances such as rush blood coagulation, antibacterial.
In existing patent of invention, Fei Hao etc. (CN103990171A), which adds bacteria cellulose film after purification, contains penta 2
In the chitosan solution of the crosslinking agents such as aldehyde, composite medical auxiliary material is prepared;Luo Xiao just waits (CN104892969A) to pass through electrostatic
Chitosan physics is coated on regenerated cellulose film surface by the mode of spraying, and chitin fiber element composite membrane is made;Shen Xinyuan etc.
(CN103550817A) by be freeze-dried be made bacteria cellulose/chitosan composite sponge, and by the sponge by adhesive,
Hot melt adhesive or heat-sensitive glue are bonded on the polypropylene nonwoven of breathable microporous, to improve its strength.Although using cellulose as
Framework material, chitosan has more research for the functional material medical dressing for composite for preparing, but still suffers from more problem.One
It is that most composite materials are membrane material, absorbency, poor air permeability.Second, complex method is mostly physical blending, dipping cladding etc., it is fine
Dimension element is only combined between chitosan by physical action, and mechanical performance is poor, in use residue easy to fall off, remains in wound
Removal is not easily cleaned in mouthful, causes the superinfection of wound.It is third, a small number of small using epoxychloropropane, glutaraldehyde, Geniposide etc.
Molecule cross-link agent is easily remained by being chemically crosslinked the cellulose-Chitosan Composites prepared, unreacted small molecule crosslinking agent
In the material, and then there is small molecule dissolution in use, cause damage to the cell of wound.
Therefore, a kind of cellulose-chitosan composite porous dressing of high intensity is developed, can not only meet to control wound to ooze
Go out liquid, avoid wound infection, keep wound moist environment, promote the basic effects such as wound healing, should also possess preferable machinery
Performance and there cannot be small molecular weight impurity dissolution.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of cellulose based on chemical crosslinking-chitosan combine dressing
And preparation method thereof, this method is simple, easily operated, and the cellulose-chitosan based on chemical crosslinking being prepared is compound to be applied
Material has good mechanicalness and pliability.
A kind of cellulose based on chemical crosslinking-chitosan combine dressing of the present invention, including epoxy silane coupling agent, fibre
Dimension element and chitosan or chitosan derivatives, have even porous net structure, chitosan or chitosan derivatives pass through epoxy
Silane coupling agent is crosslinked the surface for being evenly coated at cellulose skeleton.
The epoxy silane coupling agent is 3- (2,3- glycidoxies) propyl trimethoxy silicane, 3- (2,3- epoxies third
Epoxide) propyl-triethoxysilicane, 3- (2,3- glycidoxies) hydroxypropyl methyl dimethoxysilane, 3- (the third oxygen of 2,3- epoxies
Base) one or more in hydroxypropyl methyl diethoxy silane;Cellulose is wood pulp cellulose, bamboo cellulose, cotton cellulose
In one or more.
The cellulose is cellulose nano wire or cellulose micro wire.
The length of the cellulose nano wire is 50-1000nm, a diameter of 3-50nm of cellulose nano wire;Or cellulose
The length of micro wire is 1-10 μm, a diameter of 10-100 μm of cellulose micro wire.
The chitosan is common chitosan, the one or more in carboxymethyl chitosan, hydroxypropyl chitosan.
The deacetylation of the chitosan be more than 85%, viscosity for 100Pa.s and more than.
A kind of preparation method of the cellulose based on chemical crosslinking-chitosan combine dressing of the present invention, including:
(1) chitosan or chitosan derivatives dissolving are obtained into chitosan solution in a solvent, by chitosan solution and fibre
The plain suspension of dimension is mixed to form mixed liquor, and epoxy silane coupling agent is added in mixed liquor and is reacted, stirs, obtains mix suspending
Liquid, wherein, cellulose is 1 with the mass ratio of chitosan or chitosan derivatives:0.2-1:5, cellulose is coupled with epoxy silane
The mass ratio of agent is 1:0.5-1:6;
(2) mixing suspension for obtaining step (1) freezes, and freeze-drying, bakes, and washes successively, ethanol is washed, acetone
Wash, dry, obtain the cellulose based on chemical crosslinking-chitosan combine dressing.
Solvent is water or 1% aqueous acetic acid in the step (1);Cellulose suspension solid content is 0.8-1.6wt%;
The concentration of chitosan solution is 0.8-2wt%;The pH value of reaction is 4-9;Mixing time is 1-3h.
Freeze-drying temperature is -50--65 DEG C in the step (2), sublimation drying 20-50h;Baking temperature is
110-130 DEG C, it is 10-30min to bake the time.
Washing times are 2-5 times in the step (2), and ethanol washes number as 1-2 times, and acetone washes number as 1-3 times;Drying
Temperature is 40-60 DEG C, and drying time 3-8h, drying mode is vacuum drying.
The preparation method of a kind of cellulose based on chemical crosslinking-chitosan combine dressing of the present invention, by epoxy silane
Coupling agent is fully hydrolyzed, and the hydroxyl on silicone hydroxyl and cellulose then hydrolyzed using epoxy silane coupling agent is crosslinked, together
When the epoxide group of epoxy silane and the amino of chitosan be crosslinked, that is, cellulose and shell are gathered using epoxy silane coupling agent
Sugar is chemically crosslinked, and after freeze-dried, the cellulose based on chemical crosslinking-chitosan combine dressing is prepared.
Beneficial effect
(1) preparation method of the invention is simple, and easily operated, cost is low, environmental protection;
(2) the obtained cellulose based on the chemical crosslinking-chitosan combine dressing of the present invention have good mechanicalness and
Pliability, residue not easily to fall off, avoids the secondary pollution and damage of wound in use;Uncrosslinked epoxy silane coupling
Agent itself polycondensation forms polysilane, avoids and is caused damage using the dissolution of process small molecular to the Skin Cell of wound;
Possesses loose structure, liquid absorption amount is big and good permeability, can control wound fluid, keep wound moist environment to avoid hindering at the same time
Mouth anoxic;Chitosan is evenly coated at the surface of cellulose skeleton, by the natural antibiotic property of chitosan and coagulant property, the material
Material can promote blood coagulation and avoid wound infection, have wide practical use in medical dressing field.
Brief description of the drawings
Fig. 1 is the chemical constitution schematic diagram of the cellulose based on chemical crosslinking-chitosan combine dressing in embodiment 1;
Fig. 2 is the cellulose based on chemical crosslinking in embodiment 3-chitosan combine dressing inner scanning electron microscope
Figure;
Fig. 3 is the schematic diagram in kind of the cellulose based on chemical crosslinking-chitosan combine dressing in embodiment 2.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
(1) 0.055g chitosans (deacetylation 85%, viscosity 200Pa.s) are dissolved in 1% aqueous acetic acid
It is 1.1wt% chitosan solutions to obtain concentration, by above-mentioned chitosan solution and 5g wood pulp cellulose micro wires suspension (quality point
Number 1.1wt%) mixed liquor is mixed to form, 0.11g 3- (2,3- glycidoxy) propyl trimethoxy silicane is added to mixing
In liquid, at room temperature under the conditions of property, magnetic agitation 2h, obtains mixing suspension.
(2) mixing suspension that step (1) obtains is placed in liquid nitrogen and freezed, placed into freeze drier, freezing is dry
Dry temperature is -58 DEG C, is freeze-dried 24h, and taking-up, which is placed in vacuum drying oven, bakes 30min for 110 DEG C, washes 3 times, ethanol successively
Wash 2 times, acetone wash 3 times, be placed in vacuum drying oven 50 DEG C of drying 6h, it is compound to obtain cellulose-chitosan based on chemical crosslinking
Dressing.
Fig. 1 is the chemical constitution schematic diagram of the cellulose based on chemical crosslinking-chitosan combine dressing in the present embodiment 1,
It can be seen that chitosan is successfully chemically crosslinked on cellulose by epoxy silane coupling agent.
Embodiment 2
(1) 0.066g (is it right for specific quality) chitosan (deacetylation 95%, viscosity 400Pa.s) is dissolved in
It is 1.1wt% chitosan solutions that concentration is obtained in 1% aqueous acetic acid, by above-mentioned chitosan solution and 4g wood pulp cellulose microns
Line suspension (mass fraction 1.1wt%) is mixed to form mixed liquor, by three ethoxy of 0.055g 3- (2,3- glycidoxy) propyl group
Base silane is added in mixed liquor, and at room temperature under the conditions of property, magnetic agitation 2h, obtains mixing suspension.
(2) mixing suspension that step (1) obtains is placed in liquid nitrogen and freezed, placed into freeze drier, freezing is dry
Dry temperature is -58 DEG C, is freeze-dried 36h, and taking-up, which is placed in vacuum drying oven, bakes 10min for 120 DEG C, washes 2 times, ethanol successively
Wash 2 times, acetone wash 3 times, be placed in vacuum drying oven 60 DEG C of drying 4h, it is compound to obtain cellulose-chitosan based on chemical crosslinking
Dressing.
Fig. 3 is the schematic diagram in kind of the cellulose based on the chemical crosslinking-chitosan combine dressing of the present embodiment 2.
Embodiment 3
(1) 0.077g chitosans (deacetylation 90%, viscosity 100Pa.s) are dissolved in 1% aqueous acetic acid
It is 1.6wt% chitosan solutions to obtain concentration, by above-mentioned chitosan solution and 3g wood pulp cellulose micro wires suspension (quality point
Number 1.4wt%) mixed liquor is mixed to form, 0.22g 3- (2,3- glycidoxy) hydroxypropyl methyl dimethoxysilane is added to
In mixed liquor, at room temperature under the conditions of property, magnetic agitation 2h, obtains mixing suspension.
(2) mixing suspension that step (1) obtains is placed in liquid nitrogen and freezed, placed into freeze drier, freezing is dry
Dry temperature is -58 DEG C, is freeze-dried 24h, and taking-up, which is placed in vacuum drying oven, bakes 10min for 120 DEG C, washes 2 times, ethanol successively
Wash 2 times, acetone wash 3 times, be placed in vacuum drying oven 60 DEG C of drying 3h, it is compound to obtain cellulose-chitosan based on chemical crosslinking
Dressing.
Fig. 2 is the cellulose based on chemical crosslinking in the present embodiment 3-chitosan combine dressing inner scanning electron microscope
Figure, the cellulose based on the chemical crosslinking-chitosan combine dressing for showing to be prepared have even porous net structure, and shell gathers
Sugar is evenly coated at the surface of cellulose skeleton by the crosslinking of 3- (2,3- glycidoxy) propyl trimethoxy silicane, so as to protect
It is good to demonstrate,prove gas permeability and the absorbency of the dressing, and residue not easily to fall off, the water of 60-80 times of own wt can be adsorbed, it is acellular
Toxicity, no hemolytic, has preferable coagulant property.
Embodiment 4
(1) 0.055g carboxymethyl chitosans (deacetylation 90%, viscosity 100Pa.s) are dissolved in water to obtain dense
Spend for 1.3wt% carboxymethyl chitosan solutions, by above-mentioned chitosan solution and 6g wood pulp cellulose micro wires suspension (quality point
Number 1.1wt%) mixed liquor is mixed to form, 0.13g 3- (2,3- glycidoxy) propyl trimethoxy silicane is added to mixing
In liquid, at room temperature under the conditions of property, magnetic agitation 2h, obtains mixing suspension.
(2) mixing suspension that step (1) obtains is placed in liquid nitrogen and freezed, placed into freeze drier, freezing is dry
Dry temperature is -58 DEG C, is freeze-dried 24h, and taking-up, which is placed in vacuum drying oven, bakes 10min for 120 DEG C, washes 2 times, ethanol successively
Wash 2 times, acetone wash 3 times, be placed in vacuum drying oven 60 DEG C of drying 3h, it is compound to obtain cellulose-chitosan based on chemical crosslinking
Dressing.
Claims (10)
- A kind of 1. cellulose based on chemical crosslinking-chitosan combine dressing, it is characterised in that including epoxy silane coupling agent, Cellulose and chitosan or chitosan derivatives, have even porous net structure, chitosan or chitosan derivatives pass through ring Oxosilane coupling agent is crosslinked the surface for being evenly coated at cellulose skeleton.
- A kind of 2. cellulose based on chemical crosslinking-chitosan combine dressing described in accordance with the claim 1, it is characterised in that The epoxy silane coupling agent is 3- (2,3- glycidoxies) propyl trimethoxy silicane, 3- (2,3- glycidoxies) propyl group Triethoxysilane, 3- (2,3- glycidoxies) hydroxypropyl methyl dimethoxysilane, 3- (2,3- glycidoxies) propyl group first One or more in base diethoxy silane;Cellulose for wood pulp cellulose, bamboo cellulose, one kind in cotton cellulose or It is several.
- A kind of 3. cellulose based on chemical crosslinking-chitosan combine dressing described in accordance with the claim 1, it is characterised in that The cellulose is cellulose nano wire or cellulose micro wire.
- A kind of 4. cellulose based on chemical crosslinking-chitosan combine dressing described in accordance with the claim 3, it is characterised in that The length of the cellulose nano wire is 50-1000nm, a diameter of 3-50nm of cellulose nano wire;Or cellulose micro wire Length is 1-10 μm, a diameter of 10-100 μm of cellulose micro wire.
- A kind of 5. cellulose based on chemical crosslinking-chitosan combine dressing described in accordance with the claim 1, it is characterised in that The chitosan derivatives are carboxymethyl chitosan, one or two kinds of in hydroxypropyl chitosan.
- A kind of 6. cellulose based on chemical crosslinking-chitosan combine dressing described in accordance with the claim 1, it is characterised in that The deacetylation of the chitosan be more than 85%, viscosity for 100Pa.s and more than.
- 7. a kind of preparation method of the cellulose based on chemical crosslinking-chitosan combine dressing, including:(1) chitosan or chitosan derivatives dissolving are obtained into chitosan solution in a solvent, by chitosan solution and cellulose Suspension is mixed to form mixed liquor, and epoxy silane coupling agent is added in mixed liquor and is reacted, and stirring, obtains mixing suspension, Wherein, cellulose and the mass ratio of chitosan or chitosan derivatives are 1:0.2-1:5, cellulose and epoxy silane coupling agent Mass ratio is 1:0.5-1:6;(2) mixing suspension for obtaining step (1) freezes, and freeze-drying, bakes, and washes successively, ethanol is washed, acetone is washed, baking It is dry, obtain the cellulose based on chemical crosslinking-chitosan combine dressing.
- 8. according to a kind of preparation method of the cellulose based on chemical crosslinking-chitosan combine dressing described in claim 7, its It is characterized in that, solvent is water or 1% aqueous acetic acid in the step (1);Cellulose suspension solid content is 0.8- 1.6wt%;The concentration of chitosan solution is 0.8-2wt%;The pH value of reaction is 4-9;Mixing time is 1-3h.
- 9. according to a kind of preparation method of the cellulose based on chemical crosslinking-chitosan combine dressing described in claim 7, its It is characterized in that, freeze-drying temperature is -50--65 DEG C in the step (2), sublimation drying 20-50h;Baking temperature is 110-130 DEG C, it is 10-30min to bake the time.
- 10. according to a kind of preparation method of the cellulose based on chemical crosslinking-chitosan combine dressing described in claim 7, It is characterized in that, washing times are 2-5 times in the step (2), ethanol washes number as 1-2 times, and acetone washes number as 1-3 times; Drying temperature is 40-60 DEG C, and drying time 3-8h, drying mode is vacuum drying.
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Cited By (6)
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CN110420345A (en) * | 2019-08-02 | 2019-11-08 | 北京化工大学常州先进材料研究院 | High water absorption antibacterial anti hemorrhagic sponge |
CN110499655A (en) * | 2019-08-06 | 2019-11-26 | 浙江理工大学 | A kind of method of the natural dye dying of carboxymethyl chitosan Si modification cotton fabric |
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Cited By (9)
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CN115772348A (en) * | 2022-11-25 | 2023-03-10 | 东莞理工学院 | Full-bio-based super-hydrophilic/underwater super-oleophobic coating and preparation method thereof |
CN115772348B (en) * | 2022-11-25 | 2023-08-29 | 东莞理工学院 | Full-bio-based super-hydrophilic/underwater super-oleophobic coating and preparation method thereof |
CN116942880A (en) * | 2023-06-16 | 2023-10-27 | 广东美登新材料科技有限公司 | Ultrathin absorption core with diversion function and preparation method thereof |
CN116942880B (en) * | 2023-06-16 | 2024-05-24 | 广东美登新材料科技有限公司 | Ultrathin absorption core with diversion function and preparation method thereof |
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