CN116236607A - High-strength high-release micro-nano cellulose/sodium alginate dressing and preparation method and application thereof - Google Patents
High-strength high-release micro-nano cellulose/sodium alginate dressing and preparation method and application thereof Download PDFInfo
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- CN116236607A CN116236607A CN202310234076.XA CN202310234076A CN116236607A CN 116236607 A CN116236607 A CN 116236607A CN 202310234076 A CN202310234076 A CN 202310234076A CN 116236607 A CN116236607 A CN 116236607A
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- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 91
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 79
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 79
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 52
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 33
- 239000000835 fiber Substances 0.000 claims abstract description 32
- 239000000725 suspension Substances 0.000 claims abstract description 28
- 238000007865 diluting Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 claims abstract description 13
- 229920002674 hyaluronan Polymers 0.000 claims abstract description 13
- 229960003160 hyaluronic acid Drugs 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 13
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 229920002522 Wood fibre Polymers 0.000 claims description 19
- 239000002025 wood fiber Substances 0.000 claims description 19
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 14
- 241000196324 Embryophyta Species 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000002121 nanofiber Substances 0.000 claims description 3
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims description 2
- 229960002401 calcium lactate Drugs 0.000 claims description 2
- 239000001527 calcium lactate Substances 0.000 claims description 2
- 235000011086 calcium lactate Nutrition 0.000 claims description 2
- 239000002537 cosmetic Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 239000011121 hardwood Substances 0.000 claims description 2
- 238000000265 homogenisation Methods 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims 3
- 241000209504 Poaceae Species 0.000 claims 1
- 238000010025 steaming Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 231100000683 possible toxicity Toxicity 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000009849 vacuum degassing Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 238000007670 refining Methods 0.000 description 6
- 102000008186 Collagen Human genes 0.000 description 5
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- 239000004480 active ingredient Substances 0.000 description 5
- 229920001436 collagen Polymers 0.000 description 5
- 239000000017 hydrogel Substances 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 4
- 239000001913 cellulose Substances 0.000 description 4
- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 description 4
- 229960004989 tetracycline hydrochloride Drugs 0.000 description 4
- 229920001282 polysaccharide Polymers 0.000 description 3
- 239000005017 polysaccharide Substances 0.000 description 3
- 150000004804 polysaccharides Chemical class 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 229960001126 alginic acid Drugs 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 235000010443 alginic acid Nutrition 0.000 description 2
- 229920000615 alginic acid Polymers 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000218631 Coniferophyta Species 0.000 description 1
- 241001397809 Hakea leucoptera Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
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- 230000014759 maintenance of location Effects 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
- A61L15/225—Mixtures of macromolecular compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0212—Face masks
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/733—Alginic acid; Salts thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/8129—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers or esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers, e.g. polyvinylmethylether
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a high-strength and high-release micro-nano cellulose/sodium alginate dressing, and a preparation method and application thereof. The method comprises the following steps: the plant fiber is first defiberized, centrifuged, diluted and soaked, and the pulp is ground after soaking for a certain time; diluting the obtained slurry, and homogenizing by a high-pressure homogenizer to obtain micro-nano cellulose suspension; adding sodium alginate and hyaluronic acid into the suspension, then adding a polyvinyl alcohol solution, and uniformly stirring to obtain a mixed solution; pouring the mixed solution into a mould, and then immersing the mould into a calcium ion solution for forming to obtain the high-strength and high-release micro-nano cellulose/sodium alginate dressing. According to the invention, the micro-nano cellulose is used for promoting the rapid molding of sodium alginate, the shrinkage is reduced, and compared with a pure sodium alginate film, the added micro-nano cellulose film has higher strength and larger release amount. The preparation method solves the problems of complex production, potential toxicity and poor mechanical property of the condensation dressing in the prior art.
Description
Technical Field
The invention belongs to the field of high molecular functional materials, and particularly relates to a high-strength and high-release micro-nano cellulose/sodium alginate dressing, and a preparation method and application thereof.
Background
Hydrogels are three-dimensional network materials with high water retention properties that provide adequate moisture retention and carry sufficient amounts of active ingredients, and are of great interest for dressing applications. However, the hydrogel has poor mechanical properties, weak capability of releasing active ingredients, and unfriendly environment in the production and preparation process, which limit the application of the hydrogel on dressing.
Sodium alginate is a natural polysaccharide extracted from alginic acid, and hydrogel materials based on sodium alginate have good biocompatibility, easy degradation and high molding speed, and have many applications in the medical field. But the mechanical strength of the formed hydrogel is poor, the shrinkage is serious, and the uniformity is poor. There is an urgent need for a non-toxic bio-friendly method to solve this problem.
Most of the existing gels use alkali (for example, patent application No. 202111556373.3) or metal (for example, patent application No. 202211325914.6) as complexing agents, which pollute the environment and may be harmful to the human body.
Disclosure of Invention
In order to solve the defects and the shortcomings of the prior art, the primary purpose of the invention is to provide a preparation method of a high-strength and high-release micro-nano cellulose/sodium alginate dressing. According to the method, micro-nano cellulose is used for promoting rapid molding of sodium alginate, shrinkage is reduced, and compared with a pure sodium alginate film, the added micro-nano cellulose film has higher strength and larger release amount. The preparation method solves the problems of complex production, potential toxicity and poor mechanical property of the condensation dressing in the prior art.
Another object of the present invention is to provide a high-strength and high-release micro-nano cellulose/sodium alginate dressing prepared by the above method.
It is a further object of the present invention to provide the use of the high strength high release micro-nanocellulose/sodium alginate dressing described above.
The invention aims at realizing the following technical scheme:
the preparation method of the high-strength and high-release micro-nano cellulose/sodium alginate dressing comprises the following steps:
(1) The plant fiber is first defiberized, centrifuged, diluted and soaked, and the pulp is ground after soaking for a certain time;
(2) Diluting the slurry obtained in the step (1), and homogenizing by a high-pressure homogenizer to obtain micro-nano cellulose suspension;
(3) Adding sodium alginate and hyaluronic acid into the micro-nano cellulose suspension obtained in the step (2), then adding a polyvinyl alcohol solution, and uniformly stirring to obtain a mixed solution;
(4) Pouring the mixed solution obtained in the step (3) into a mould, and then immersing the mould into a calcium ion solution for forming to obtain a crosslinked film-forming micro-nano cellulose/sodium alginate film, namely the high-strength and high-release micro-nano cellulose/sodium alginate dressing.
Preferably, the plant fiber of step (1) comprises at least one of needle-leaf wood fiber, hardwood fiber, graminaceous fiber, bast fiber, seed hair fiber and leaf fiber. The present invention preferably uses needle wood fibers.
Preferably, the speed of the centrifugation in the step (1) is 3000-10000r/min, and the centrifugation time is 10-30min.
Preferably, the dilution in the step (1) means that the conifer fiber is diluted to 7-15wt%.
Preferably, the soaking time in the step (1) is 12-24 hours.
Preferably, the refining in the step (1) means treatment by using a PFI refiner, and the refining revolution is 30000-100000r, and is used for cutting and microfibrillating the needle-leaved wood fibers.
Preferably, step (2) dilutes the slurry to a fiber concentration of 0.1-1.5wt%; the homogenization times are 5-30 times.
Preferably, the micro-nano fiber in the step (2) is 10nm-100nm wide, and the length-diameter ratio is more than 100.
Preferably, the homogenizing step (2) further comprises spin-evaporating the suspension at 40 ℃ under 2000Pa low vacuum and 180r/min until the concentration of the micro-nano cellulose is 0.8wt%.
Preferably, in the mixed solution in step (3): the concentration of the micro-nano cellulose is 0.3-1.5wt%, the concentration of the sodium alginate is 1-3wt%, the concentration of the hyaluronic acid is 0.1-0.25wt%, and the concentration of the polyvinyl alcohol is 1wt%.
Preferably, the concentration of the polyvinyl alcohol solution in the step (3) is 5-20wt%.
Preferably, in the step (4), the mixed solution is subjected to vacuum defoaming, and then poured into a mold.
Further preferably, the vacuum degassing is performed at 0.1 MPa.
Preferably, the concentration of the calcium ion solution in the step (4) is 0.5-2wt% and the molding time is 5-20min.
Preferably, the calcium ion solution in the step (4) comprises calcium chloride, calcium sulfate, calcium lactate or the like.
The strength of the high-strength high-release micro-nano cellulose/sodium alginate dressing is 40-140Kpa, the elongation is 70-260%, and the release rate in one hour is more than 50%.
The high-strength and high-release micro-nano cellulose/sodium alginate dressing can be applied to medical dressing and cosmetic mask.
Compared with the prior art, the invention has the following advantages:
(1) The materials used by the invention are low in price and rich in reserves. Cellulose is the most abundant polysaccharide in the world, sodium alginate is natural polysaccharide extracted from marine plants, and has the characteristics of biodegradability, good biocompatibility and the like, and the prepared material has very wide application scenes.
(2) The micro-nano cellulose with high length-diameter ratio prepared by a mechanical method has the characteristics of high specific surface area, high strength and low density, and meanwhile, the surface contains rich hydroxyl groups, so that hydrogen bonds can be formed with alginic acid, the strength of a sodium alginate film is remarkably improved, the formation in a calcium ion solution is promoted, the shrinkage of the film in the formation process is reduced, and the release efficiency of the film is increased, so that the micro-nano cellulose is very important for dressing.
(3) The preparation method of the invention is easy to operate, does not produce waste chemicals, is environment-friendly and is easy to realize industrialization.
Drawings
Fig. 1 is an electron microscopic image of the cellulose raw material used in example 1.
Fig. 2 is an electron microscope image of the micro-nano cellulose prepared in example 1.
FIG. 3 shows different micro-nanocellulose (CNF), polyvinyl alcohol (PVA) and sodium alginate at different concentrations of CaCl 2 Soaking and molding, and shrinking in the molding process.
Fig. 4 is a drawing of different films. The tensile strength test method in the figure: the film width was 10mm, the film length was 30mm, and the stretching speed was 1mm/min.
FIG. 5 is a photograph of four repeated stretches of CNF/SA-0.5wt% film, showing a tensile strength test method: the film width is 10mm, the film length is 30mm, the stretching speed is 1mm/min, the first stretching is carried out, the stretching rate is 30 percent, the original position is returned, the second stretching is carried out, and the stretching is carried out until the stretching rate is 60 percent, and the original position is returned. Break during the third stretching. In the figure, CNF/SA-0.5wt% -1 means stretching for the first time, CNF/SA-0.5wt% -2 means stretching for the second time, and CNF/SA-0.5wt% -3 means stretching for the third time.
FIG. 6 is a photograph of four repeated stretches of CNF/PVA/SA-0.5wt% film, showing a tensile strength test method: the film width is 10mm, the film length is 30mm, the stretching speed is 1mm/min, the first stretching is carried out, the stretching rate is 30 percent, the original position is returned, the second stretching is carried out, and the stretching is carried out until the stretching rate is 60 percent, and the original position is returned. And (3) stretching for the third time, breaking in the process, returning to the original position after the stretching until the elongation is 90%, and stretching for the fourth time. In the figure, CNF/PVA/SA-0.5wt% -1 means stretching for the first time, CNF/PVA/SA-0.5wt% -2 means stretching for the second time, CNF/PVA/SA-0.5wt% -3 means stretching for the third time, and CNF/PVA/SA-0.5wt% -4 means stretching for the fourth time.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; treatment with a PFI refiner at 60000 refining revolutions r 。
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 5g of polyvinyl alcohol was weighed into 45g of water and stirred at 200r/min for half an hour under a water bath at 98℃to obtain a completely dissolved polyvinyl alcohol solution.
1.8g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of a 0.8wt% micro-nanocellulose suspension, and stirred uniformly at room temperature. Then 10g of polyvinyl alcohol solution is weighed and added into the micro-nano cellulose suspension, and the mixture is stirred for 1h at 200r/min to obtain a uniformly mixed suspension. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain the crosslinked film-forming micro-nano cellulose/sodium alginate film, and the marking number is CNF/SA/PVA-0.5wt%.
Example 2
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; the pulp was processed using a PFI refiner at 60000r.
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 5g of polyvinyl alcohol was weighed into 45g of water, and stirred at 200r/min for half an hour under a water bath at 100℃to obtain a completely dissolved polyvinyl alcohol solution.
1.5g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of a 0.8wt% micro-nanocellulose suspension, and stirred uniformly at room temperature. Then 10g of polyvinyl alcohol solution is weighed and added into the micro-nano cellulose suspension, and the suspension is obtained after stirring for 1h at 200 r/min. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, the culture dish is slowly immersed into a 1wt% calcium chloride solution for 10min, and the crosslinked film-forming micro-nano cellulose/sodium alginate film is obtained, and the sample number is CNF/SA/PVA-1wt%.
Example 3
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; the pulp was processed using a PFI refiner at 60000r.
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 5g of polyvinyl alcohol was weighed into 45g of water, and stirred at 200r/min for half an hour under a water bath at 100℃to obtain a completely dissolved polyvinyl alcohol solution.
1.5g of sodium alginate and 0.1g of tetracycline hydrochloride are weighed and dissolved in 100ml of 0.8wt% micro-nano cellulose suspension, and stirred uniformly at room temperature. Then 10g of polyvinyl alcohol solution is weighed and added into the micro-nano cellulose suspension, and the suspension is obtained after stirring for 1h at 200 r/min. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, the culture dish is slowly immersed into a 1wt% calcium chloride solution for 10min, and the crosslinked film-forming micro-nano cellulose/sodium alginate film is obtained, and the sample number CNF/SA/PVA-0.5wt% -T is recorded.
Example 4
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; the pulp was processed using a PFI refiner at 60000r.
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 5g of polyvinyl alcohol was weighed into 45g of water, and stirred at 200r/min for half an hour under a water bath at 100℃to obtain a completely dissolved polyvinyl alcohol solution.
1.5g of sodium alginate and 0.1g of collagen are weighed and dissolved in 100ml of 0.8wt% micro-nano cellulose suspension, and stirred uniformly at room temperature. Then 10g of the polyvinyl alcohol solution in the second step is weighed and added into the micro-nano cellulose suspension, and the mixture is stirred for 1h at 200r/min to obtain a uniformly mixed suspension. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain the crosslinked film-forming micro-nano cellulose/sodium alginate film CNF/SA/PVA-0.5wt% -C.
Example 5
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; treatment with a PFI refiner at 60000 refining revolutions r 。
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 5g of polyvinyl alcohol was weighed into 45g of water, and stirred at 200r/min for half an hour under a water bath at 100℃to obtain a completely dissolved polyvinyl alcohol solution.
1.5g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of a 0.8wt% micro-nanocellulose suspension, and stirred uniformly at room temperature. Then 10g of polyvinyl alcohol solution is weighed and added into the micro-nano cellulose suspension, and the suspension is obtained after stirring for 1h at 200 r/min. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 6g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into a 1wt% calcium chloride solution for 10min, so that the crosslinked film-forming micro-nano cellulose/sodium alginate film is obtained, and the number is CNF/SA (1.5%)/PVA-1 wt%.
Comparative example 1
And taking the polyvinyl alcohol without micro-nano cellulose and the sodium alginate film as a control, and observing film shrinkage and strength change conditions.
Step (1): 7.5g of polyvinyl alcohol was weighed and added to 42.5g of water, and stirred at 200r/min for 1 hour in a water bath at 98℃to obtain a completely dissolved polyvinyl alcohol solution.
Step (2): 1.8g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of pure water, and stirred uniformly at room temperature. Then, 10g of a polyvinyl alcohol solution was weighed, added into the solution, and stirred for 1 hour at 200r/min to obtain a uniformly mixed suspension. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (3): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain the crosslinked film-forming micro-nano cellulose/sodium alginate film, and the mark number is SA/PVA-0.5wt%.
Comparative example 2
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; treatment with a PFI refiner at 60000 refining revolutions r 。
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nano cellulose is steamed to the concentration of 0.8wt% by rotating under the conditions of 40 ℃ and 2000Pa low vacuum and 180 r/min.
Step (3): 1.5g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of a 0.8wt% micro-nanocellulose suspension, and stirred uniformly at room temperature. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of liquid after vacuum defoamation is poured into a culture dish with the diameter of 8.5cm, the culture dish is slowly immersed into a 1wt% calcium chloride solution for 10min, and the micro-nano cellulose/sodium alginate film which is completely crosslinked and formed is obtained, and the sample number is CNF/SA-1wt%.
Comparative example 3
And taking the micro-nano cellulose without polyvinyl alcohol and the sodium alginate film as a control, and observing film shrinkage and strength change conditions.
Step (1): fluffing the needle leaf wood fiber in advance by a tile Li Dajiang machine, centrifuging at 4000r/min for 15min, diluting the obtained needle leaf wood fiber to 10wt%, and soaking for 12h; treatment with a PFI refiner at 60000 refining revolutions r 。
Step (2): and diluting the obtained fiber until the fiber concentration is 0.3 weight percent, and homogenizing for 5 times by a high-pressure homogenizer to obtain uniform and fine micro-nano cellulose. The diameter of the micro-nano cellulose is 20-50nm, and the length-diameter ratio is 150-200. The micro-nanocellulose was spin-distilled to a concentration of 0.8wt% at 40 ℃,2000Pa low vacuum, 180 r/min.
Step (3): 1.8g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of a 0.8wt% micro-nanocellulose suspension, and stirred uniformly at room temperature. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (4): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain the crosslinked film-forming micro-nano cellulose/sodium alginate film, and the mark number is CNF/SA-0.5wt%.
Comparative example 4
And taking a sodium alginate film without polyvinyl alcohol and micro-nano cellulose as a control, and observing film shrinkage and strength change conditions.
Step (1): 1.8g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of pure water, and stirred uniformly at room temperature. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (2): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain the crosslinked film-forming micro-nano cellulose/sodium alginate film, and the mark number is SA-0.5wt%.
Comparative example 5
And taking the polyvinyl alcohol without the micro-nano cellulose and the sodium alginate film as a control, and observing the release condition of the tetracycline hydrochloride.
Step (1): 7.5g of polyvinyl alcohol was weighed and added to 42.5g of water, and stirred at 200r/min for 1 hour in a water bath at 98℃to obtain a completely dissolved polyvinyl alcohol solution.
Step (2): 1.8g of sodium alginate and 0.1g of hyaluronic acid were weighed and dissolved in 100ml of pure water, and stirred uniformly at room temperature. Then, 10g of a polyvinyl alcohol solution was weighed, added into the solution, and stirred for 1 hour at 200r/min to obtain a uniformly mixed suspension. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (3): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain a crosslinked film-forming polyvinyl alcohol/sodium alginate film, and SA/PVA-0.5wt% -T is recorded.
Comparative example 6
And taking the polyvinyl alcohol without the micro-nano cellulose and the sodium alginate film as a control, and observing the release condition of the collagen.
Step (1): 7.5g of polyvinyl alcohol was weighed and added to 42.5g of water, and stirred at 200r/min for 1 hour under a water bath at 98℃to obtain a dissolved polyvinyl alcohol solution.
Step (2): 1.8g of sodium alginate and 0.1g of collagen are weighed and dissolved in 100ml of pure water, and stirred uniformly at room temperature. Then, 10g of a polyvinyl alcohol solution was weighed, added into the solution, and stirred for 1 hour at 200r/min to obtain a uniformly mixed suspension. The resulting liquid was subjected to vacuum degassing at 0.1 MPa.
Step (3): 9g of the vacuum defoamed liquid is poured into a culture dish with the diameter of 8.5cm, and the culture dish is slowly immersed into 0.5wt% of calcium chloride solution for 10min, so as to obtain a cross-linked film-forming polyvinyl alcohol/sodium alginate film, and the number SA/PVA-0.5wt% -C is recorded.
To evaluate the release of the active ingredient from the film, the release of the active ingredient was simulated with tetracycline hydrochloride. The sample was placed in 100ml PBS buffer, shaken at 50r/min on an air shaker, 4ml of slow release solutions were taken at 15, 30, 45 and 60min, respectively, and detected at a wavelength of 360nm using an ultraviolet-visible photometer. As described in table 1, the release amount was already close to or even over 50% in the first 1h, whereas the release rate was only 38.29% in the sample of comparative example 2, to which CNF was not added. The release performance of the nano-cellulose is obviously improved compared with that of the nano-cellulose which is not added.
Table 1 two parallel samples of sample-CNF/SA/PVA-0.5 wt% -T from example 3 and sample SA/PVA-0.5wt% -T from comparative example 5 were each subjected to tetracycline hydrochloride release.
And (II) simulating the release of the active ingredients by using collagen in order to further evaluate the release conditions of the membrane on different ingredients. The sample was placed in 100ml PBS buffer and shaken at 50r/min on an air shaker, 4ml of slow release solutions were taken at 15, 30, 45 and 60min, respectively, and detected at a wavelength of 230nm using an ultraviolet-visible photometer. As described in Table 2, the release amount was already over 50% in the first 1 hour, and the release effect was excellent. The release rate was investigated in comparative example 6, but the samples were broken when PVA/SA without nanofibers was immersed in water, and as a result, failed to use.
TABLE 2 collagen Release from two parallel samples-CNF/SA/PVA-0.5 wt% to C obtained in example 4
(III) figure 1 shows how the film shrinks during the six preparation processes of the hybrid film. The positive effect of the addition of the micro-nano cellulose and the polyvinyl alcohol on the film forming shrinkage rate and the influence of the calcium ion concentration on the film shrinkage rate during forming are explored. Table 3 specifically describes the case expressed in FIG. 3, where the shrinkage of pure Sodium Alginate (SA) film was as high as 42.12% and the molding effect was poor after 10min of immersion. The shrinkage rate was reduced to 24.12% after only polyvinyl alcohol (PVA) was added, but the shrinkage rate of the film was reduced to 18.94% by adding micro-nano Cellulose (CNF) under the same molding conditions, and the shrinkage rate was only 7.65% when micro-nano cellulose and polyvinyl alcohol were simultaneously added, and the surface of the film was smooth and flat. The 0.5wt% molded film strength and toughness are better compared to 0.5wt% and 1wt% molded calcium chloride.
The tensile profile of the film formed in the different calcium ions illustrated in figure 3 demonstrates that 0.5wt% formed film is better. Meanwhile, experiments show that the tensile strength and toughness of the film added with the polyvinyl alcohol are reduced relative to those of the film which is not added with the polyvinyl alcohol. The data of figures 4 and 5 demonstrate that the addition of polyvinyl alcohol favors hydrogen bond recombination during continuous pulling, and that superior toughness and strength is reversed after repeated stretching.
TABLE 3 shrinkage of samples from examples 1,2 and comparative examples 1-4
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the high-strength and high-release micro-nano cellulose/sodium alginate dressing is characterized by comprising the following steps of:
(1) The plant fiber is first defiberized, centrifuged, diluted and soaked, and the pulp is ground after soaking for a certain time;
(2) Diluting the slurry obtained in the step (1), and homogenizing by a high-pressure homogenizer to obtain micro-nano cellulose suspension;
(3) Adding sodium alginate and hyaluronic acid into the micro-nano cellulose suspension obtained in the step (2), then adding a polyvinyl alcohol solution, and uniformly stirring to obtain a mixed solution;
(4) Pouring the mixed solution obtained in the step (3) into a mould, and then immersing the mould into a calcium ion solution for forming to obtain the high-strength and high-release micro-nano cellulose/sodium alginate dressing.
2. The method for preparing a high-strength high-release micro-nanocellulose/sodium alginate dressing according to claim 1, wherein the plant fibers in step (1) comprise at least one of needle-leaved wood fibers, hardwood fibers, gramineae fibers, bast fibers, seed hair fibers and leaf fibers;
the speed of the centrifugation in the step (1) is 3000-10000r/min, and the centrifugation time is 10-30min;
the dilution in the step (1) means that the needle leaf wood fiber is diluted to 7-15wt%;
the soaking time in the step (1) is 12-24 hours;
the step (1) of pulping refers to the process of using a PFI pulping machine, and the pulping revolution is 30000-100000r.
3. The method for preparing the high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein the step (2) is to dilute the slurry to the fiber concentration of 0.1-1.5wt%; the homogenization times are 5-30 times;
and (3) the micro-nano fiber in the step (2) is 10nm-100nm wide, and the length-diameter ratio is more than 100.
4. The method for preparing the high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein the homogenized material in the step (2) further comprises the step of spin-steaming the suspension at 40 ℃ and 2000Pa low vacuum and 180r/min until the concentration of the micro-nano cellulose is 0.8wt%.
5. The method for preparing the high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein in the mixed solution in the step (3): the concentration of the micro-nano cellulose is 0.3-1.5wt%, the concentration of the sodium alginate is 1-3wt%, the concentration of the hyaluronic acid is 0.1-0.25wt%, and the concentration of the polyvinyl alcohol is 1wt%.
6. The method for preparing the high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein in the step (4), the mixed solution is firstly subjected to vacuum defoaming and then poured into a die.
7. The method for preparing the high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein the concentration of the calcium ion solution in the step (4) is 0.5-2wt% and the molding time is 5-20min.
8. The method for preparing a high-strength and high-release micro-nano cellulose/sodium alginate dressing according to claim 1, wherein the calcium ion solution in the step (4) comprises calcium chloride, calcium sulfate or calcium lactate.
9. A high strength high release micro-nanocellulose/sodium alginate dressing, characterized in that it is prepared by the method of any one of claims 1-8.
10. The use of the high-strength high-release micro-nanocellulose/sodium alginate dressing of claim 9 in the preparation of medical dressing or cosmetic mask.
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