CN104436281A - Preparation method of porous sodium alginate nano-fiber wound dressing - Google Patents
Preparation method of porous sodium alginate nano-fiber wound dressing Download PDFInfo
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Abstract
The invention relates to a preparation method of a porous sodium alginate nano-fiber wound dressing material. The method comprises the following steps: preparing a spinning solution by dissolving sodium alginate and a water-soluble polymer as basic raw materials and a thermal decomposition foaming agent as a porogenic agent in water according to a certain mass ratio, preparing sodium alginate composite nano-fiber by adopting an electrostatic spinning technology, then performing thermal treatment on the nano-fiber at a certain temperature to decompose the foaming agent, and forming holes in and on the surface of the fiber to obtain a porous sodium alginate nano-fiber membrane; and performing chemical crosslinking on the porous sodium alginate nano-fiber membrane in an ethanol solution of CaCl2 to obtain porous sodium alginate nano-fiber wound dressing. The method disclosed by the invention has the advantages of simple preparation process, controllable process conditions and easiness in control of material structure and performance; and the material prepared by the method disclosed by the invention has high specific surface area and porosity, and excellent water absorption and water holding performance, and can be used as the medical wound dressing.
Description
technical field
The present invention relates to a kind of preparation method of porous sodium alginate nano fiber Wound dressing, belong to hygienic material technical field.
background technology
Medical wounded surface dressing is as clinical biochemical materials'use, and its research and development is a hot issue always.Current domestic existing Wound dressing mainly comprises common plant fiber, carboxymethyl cellulose class, chitosan etc.; But ubiquity product category and function singleness, do not form the problems such as series of products, functional defect, be therefore necessary to research and develop Novel wound dressing and performance and the clinical efficacy of giving its excellence.A large amount of basic research about wound surface and clinical treatment demonstrate as wound surface provides suitable moist environment to be conducive to the healing of wound in recent decades.New pattern compress can keep the moistening healing that can promote again wound of wound surface.At present, new pattern compress uses comparatively universal in developed country, and domestic also beginning is gradually applied in the treatment of various wound surface.
Sodium alginate is the polysaccharide material refined from seaweed plants.Alginic acid fibre has high moisture absorption and becomes the excellent specific property such as colloidality, high oxygen permeability, biocompatibility, biodegradation absorbability, macroion adsorptivity.When alginic acid fibre acts on wound-contacting layer, the interphase interaction of it and wound and produce sodium alginate, calcium alginate gel.This gel has hydrophilic, and oxygen can be made to pass through and antibacterial not by.Compared with traditional dressing, alginic acid dressing hygroscopicity is high, and anthemorrhagic performance is good, good biocompatibility, can promote wound healing, wound again more after can without removing sorely.
The manufacture of current nanofiber one of is the focus of world attention.Nanofiber has less diameter and larger specific surface area, and thus tool has been widely used.The non-woven fabrics utilizing nanofiber to make has the feature of highly-breathable, adds nanofiber and has large surface area, is commonly used to make medical dressing to promote that wound restores.Nano fibrous membrane has high porosity, is conducive to the absorption of wound fluid, and oxygen easily through, be conducive to wound tissue Cellular respiration, the growth of epithelial tissue and regeneration, accelerate the healing of wound.Because sodium alginate nano fiber is in the potential using value of biomedical sector, caused the dense research interest of people in recent years.It take sodium alginate as the nano fiber scaffold material of substrate that publication number 101011597 discloses a kind of, introduces polyethylene glycol oxide or polyvinyl alcohol has prepared sodium alginate nano fiber timbering material by the method for electrostatic spinning.Publication number 101230150 discloses a kind of preparation method of pure Na-alginate micro/nano fibrous membrane material, a kind of modifier-polyol glycerol of solvent type strong polarity is introduced in the aqueous solution of sodium alginate, the physical property of sodium alginate aqueous solution is effectively regulated by the strong polarity of this compound and low surface tension etc., thus realize sodium alginate soln from spinning spinnable transformation, and obtain uniform and smooth pure sodium alginate nano fiber membrane material.
Xie Hong etc. are that the calcium chloride/ethanol solution of 3% is for cross-linking agent with mass fraction, polyvinyl alcohol/sodium alginate the electrostatic spinning nano fiber being loaded with moxifloxacin hydrochloride is cross-linked, drug-loading fibre in drug release in vitro result of study show: along with the increase of crosslinking time, drug releasing rate slows down.Concluding that employing calcium chloride/ethanol solution is that the water-fast and swelling behavior of the polyvinyl alcohol/sodium alginate electrostatic spinning fiber of cross-linking agent modification is good, being more suitable for feeling embarrassed healing and have the dressing of the wound of transudate.Ice filling ice etc. by sodium alginate and Polyethylene Glycol (PEG) blended, be dissolved in water, prepared sodium alginate composite nano fiber through electrospinning process.
Sodium alginate nano fiber prepared by above-mentioned electrospinning process is real core, and the porosity of material is difficult to further raising, and prepares the high material of porosity and be conducive to increasing permeability, improves material absorbency, is beneficial to promotion wound healing.Electrostatic spinning technique and foaming agent pore methods combining are got up, in nanofiber surface and inner pore on the basis of preparing nanofiber, the nano-fiber material with more high porosity can be obtained, this a kind of method that will be effective raising material porosity, namely the present invention proposes under this technical background, inventor is found by research, the combination technique that electrospinning process and foaming agent pore methods combining get up can prepare the porous sodium alginate nano fiber of high porosity, this material has water suction and the water retention property of high specific surface area and porosity and excellence, can be used as Medical wounded surface dressing to use.
summary of the invention
The object of the invention is, in order to be to provide a kind of preparation method of porous sodium alginate nano fiber Wound dressing, sodium alginate nano fiber material is made to possess high-ratio surface sum porosity, high water suction, moisture holding capacity, good biocompatibility and anthemorrhagic performance; Meanwhile, overcome the mechanical deficiencies that calcium alginate henatischesis fiber weakness is large, be beneficial to wound tissue Cellular respiration, the growth of epithelial tissue and regeneration, accelerate the healing of wound.
Technical scheme of the present invention is, the present invention with sodium alginate and water-soluble polymer for base stock, thermal decomposition of blowing agent is as porogen, be dissolved in water in certain mass ratio, preparation spinning solution, adopt electrostatic spinning technique to prepare sodium alginate composite nano fiber, then heat treatment nanofiber at a certain temperature, foaming agent is decomposed, in fibrous inside and surperficial pore, obtains porous sodium alginate nano fiber film; By porous sodium alginate nano fiber film at CaCl
2alcoholic solution in carry out chemical crosslinking, obtain porous sodium alginate nano fiber Wound dressing material.
Porous sodium alginate nano fiber Wound dressing preparation method of the present invention is carried out as follows
(1) preparation of solution
Sodium alginate and water-soluble polymer and thermal decomposition of blowing agent are dissolved in water, are made into the spinning solution of homogeneous transparent.Wherein the content of sodium alginate is between 0.5%-4% (wt/v), preferred 1%-2%, water-soluble polymer content between 4%-12% (wt/v), preferred 6%-9%, foaming agents content is the 0.2%-5% (wt/w) of raw material components, preferred 0.5%-2%.
Described water-soluble polymer can be synthesize macromolecule as polyvinyl alcohol, polyethylene glycol oxide, Polyethylene Glycol etc., also can be that natural polymer is as gelatin, chitosan, collagen protein etc.
Described thermal decomposition of blowing agent can be inorganic matter as ammonium bicarbonate, sodium bicarbonate also can be that Organic substance is as azo-bis-iso-dimethyl etc.
(2) electrospun nanofibers
Electrostatic spinning process is: load in the device for storing liquid of constant temperature by the mixture solution containing sodium alginate and water-soluble polymer and thermal decomposition of blowing agent of step (1), device for storing liquid connection traffic pump, device for storing liquid is connected with spinning head by four fluorine tube, distance between adjustment spinning head and the catcher of ground connection, Jian opens high voltage power supply, turn-on flow rate pump, injection stream is mapped on the catcher of certain translational speed, obtains sodium alginate composite nano-fiber membrane material.
Described electrospinning device is mainly made up of high voltage power supply, charging gear, injection apparatus, gathering-device four part, and voltage is between 15KV-40KV, and solution flow rate is between 0.3ml/h-9ml/h, and receiving range is between 5cm-25cm.Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.
(3) nanofiber heat treatment prepares porous nano-fibre
Material heat treatment process is: the sodium alginate composite nano-fiber membrane material containing thermal decomposition of blowing agent of step (2) is placed in air dry oven, temperature is regulated to cause the decomposition temperature of foaming agent, heat treatment 24-48 hour, foaming agent is decomposed and produces gas, at nanofiber, inner and surperficial pore, obtains porous sodium alginate nano fiber film.
Described heat treatment temperature is selected according to the character of foaming agent, between 50 DEG C-100 DEG C.
(4) porous nano-fibre chemical crosslinking
The method of chemical crosslinking provides the polymer nano fibrous membrane materials of the different degree of cross linking, and the porous sodium alginate nano fiber membrane material that step (3) obtains is placed in CaCl
2alcoholic solution in, normal temperature crosslinked 10-48 hour, then absolute ethanol washing is until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven, obtains porous sodium alginate nano fiber Wound dressing material.
Wherein porous sodium alginate nano fiber membrane material and CaCl
2the weight of alcoholic solution and volume ratio be 1:20-2000 (as g/ml), CaCl
2concentration is in ethanol 0.5%-4%g/L.
Compared with prior art, the invention has the beneficial effects as follows:
The invention provides a kind of method that combination technique adopting electrospinning process and foaming agent pore methods combining to get up prepares porous sodium alginate nano fiber Wound dressing material.
The present invention obtains porous sodium alginate nano fiber Wound dressing material, there is water suction and the water retention property of high-ratio surface sum porosity and excellence, the weight of nearly own wt 14 times of water can be absorbed, and moisture holding capacity reaches 10 hours under 37 ° of C, for wound healing acceleration provides good wet environment.
The present invention obtain porous sodium alginate nano fiber Wound dressing there is good biocompatibility and cellular affinity, growth and the regeneration of wound tissue Cellular respiration, epithelial tissue can be promoted, accelerate the healing of wound.The present invention obtains porous sodium alginate nano fiber, with can rapid adsorption thrombin Fibrinogen and discharge Ca during contacting blood
2+, the carrying out of intrinsic coagulation mechanism can be accelerated.
The present invention uses special process to prepare porous sodium alginate nano fiber Wound dressing, overcome the problem of strong, the ventilative or drain of fragility that existing alginic acid fibre medical dressing exists, moisture sorption effect difference, can be various skin wound and different repairing phase provides multi-functional wound dressing, there is sterilization, antiinflammatory, stop blooding, relieve the pain, reduce and infect and the effects such as Promotive union.
Material preparation process of the present invention is simple, and process conditions are controlled, and material structure and performance easily control.The porous sodium alginate nano fiber of preparation can be used as Wound dressing and uses.
Porous sodium alginate nano fiber of the present invention has water suction and the water retention property of high specific surface area and porosity and excellence, can be used as Medical wounded surface dressing and uses.
accompanying drawing explanation
Fig. 1 is FB(flow block) of the present invention;
Fig. 2 is porous sodium alginate nano fiber picture in kind prepared by the inventive method;
Fig. 3 is porous sodium alginate nano fiber electromicroscopic photograph prepared by the inventive method.
Detailed description of the invention
Embodiment 1
Take 8 grams of PVA and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PVA dissolve formation clear solution, and add 1 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.18 gram of ammonium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 50 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 2
Take 10 grams of gelatin and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes Gelatin form clear solution, adds 1 gram of sodium alginate after being cooled to room temperature, and magnetic agitation 1h dissolves and forms clear solution, then add 0.22 gram of ammonium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 50 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 3
Take 10 grams of PEO and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PEO dissolve formation clear solution, and add 1 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.22 gram of ammonium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 50 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 4
Take 8 grams of PVA and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PVA dissolve formation clear solution, and add 1 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.18 gram of sodium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 80 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 5
Take 8 grams of PVA and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PVA dissolve formation clear solution, and add 0.5 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.18 gram of sodium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 80 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 6
Take 8 grams of PVA and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PVA dissolve formation clear solution, and add 1 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.5 gram of ammonium bicarbonate, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 50 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Embodiment 7
Take 8 grams of PVA and add 100ml deionized water, stirring 2h at 80 DEG C of water-bath lower magnetic forces makes PVA dissolve formation clear solution, and add 1 gram of sodium alginate after being cooled to room temperature, magnetic agitation 1h dissolves and forms clear solution, then add 0.18 gram of azo-bis-iso-dimethyl, stirring and dissolving obtains spinning liquid.
Spinning liquid is loaded in device for storing liquid, utilize electrostatic spinning apparatus to prepare sodium alginate composite nano-fiber membrane material.Spinning condition: voltage 30KV, solution flow rate 3ml/h, distance 10cm.
Prepared sodium alginate composite nano-fiber membrane material vacuum drying 2 days in vacuum drying oven.Then proceed in air dry oven, heat treatment 24h at 70 DEG C, obtain porous sodium alginate nano fiber film.
Porous sodium alginate nano fiber membrane material is placed in containing 3%CaCl
2alcoholic solution in (material and solution quality volume ratio are 1:100g/ml), normal temperature crosslinked 24h, absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.Prepared material has loose structure.
Claims (7)
1. the preparation method of a porous sodium alginate nano fiber Wound dressing material, it is characterized in that, described method with sodium alginate and water-soluble polymer for base stock, thermal decomposition of blowing agent, as porogen, is dissolved in water in certain mass ratio, preparation spinning solution, electrostatic spinning technique is adopted to prepare sodium alginate composite nano fiber, then heat treatment nanofiber makes foaming agent decompose at a certain temperature, in fibrous inside and surperficial pore, obtains porous sodium alginate nano fiber film; By porous sodium alginate nano fiber film at CaCl
2alcoholic solution in carry out chemical crosslinking, obtain porous sodium alginate nano fiber Wound dressing material.
2. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 1, it is characterized in that, described water-soluble polymer can be synthesize macromolecule as polyvinyl alcohol, polyethylene glycol oxide, Polyethylene Glycol, also can be that natural polymer is as gelatin, chitosan, collagen protein.
3. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 1, it is characterized in that, described thermal decomposition of blowing agent can be inorganic matter as ammonium bicarbonate, sodium bicarbonate also can be that Organic substance is as azo-bis-iso-dimethyl.
4. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 1, it is characterized in that, in described spinning solution, component comprises sodium alginate, water-soluble polymer and foaming agent by weight, in solution, the content of sodium alginate is between 0.5%-4%, water-soluble polymer content is between 4%-12%, and foaming agents content is the 0.2%-5% of raw material components; Described heat treatment temperature is between 50 DEG C-100 DEG C.
5. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 1, it is characterized in that, composition by weight in described spinning solution, the content of sodium alginate is preferably %-2%; Water-soluble polymer content is preferably 6%-9%; Foaming agents content is preferably 0.5%-2%.
6. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 1, it is characterized in that, porous sodium alginate nano fiber membrane material is placed in CaCl by described Chemical Crosslinking Methods
2alcoholic solution in, normal temperature crosslinked 10-48 hour, then with absolute ethanol washing until the cross-linking agent of remnants washes away completely, then vacuum drying 2 days in vacuum drying oven.
7. the preparation method of a kind of porous sodium alginate nano fiber Wound dressing material according to claim 6, is characterized in that, in described chemical crosslinking, and described porous sodium alginate nano fiber membrane material and CaCl
2the weight of alcoholic solution and volume ratio be 1:20-2000(g/ml); CaCl
2concentration is in ethanol 0.5%-4%(g/L).
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