CN105586716A - High-content sodium alginate nanofiber membrane and electrostatic spinning manufacturing method thereof - Google Patents
High-content sodium alginate nanofiber membrane and electrostatic spinning manufacturing method thereof Download PDFInfo
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- CN105586716A CN105586716A CN201410576228.5A CN201410576228A CN105586716A CN 105586716 A CN105586716 A CN 105586716A CN 201410576228 A CN201410576228 A CN 201410576228A CN 105586716 A CN105586716 A CN 105586716A
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Abstract
The invention provides a high-content sodium alginate nanofiber membrane and an electrostatic spinning manufacturing method thereof. The material is formed by sodium alginate or sodium alginate and polyvinyl alcohol, wherein the absolute content of the sodium alginate is 42.5 wt% to 100 wt%, and average diameter of the fiber is 100 nm to 150 nm. A solvent used in a preparation process of an electrostatic spinning solution is deionized water, and a surfactant is TX-100 which is certificated by US Food and Drug Administration. The manufacturing method is simple and feasible, and the high-content sodium alginate nanofiber membrane is not added with any hazardous substance. The manufactured sodium alginate nanofiber membrane is characterized by high content of sodium alginate, thin average diameter, and high porosity. The sodium alginate nanofiber membrane can be applied in the fields of wound dressing and tissue engineering (for example, a support material), etc.
Description
Technical field
The invention belongs to polymeric material field, relate to specifically a kind of high-load sodium alginate nano fiber film and electrostatic spinning preparation method thereof.
Background technology
Sodium alginate is a kind of natural anionic water-soluble polysaccharide extracting from natural brown alga, and by having two kinds of monomer beta-D-mannuronic acids (M) and α-L-guluronic acid (G) to form, its structure is similar to polysaccharide component in extracellular matrix. Sodium alginate has good biocompatibility and degradability, has no side effect and can not cause antigen-reactive, and it has demonstrated and has been applicable to various organizational project application, as skin, and cartilage, bone, nerve fiber etc.
N cell epimatrix in tissue mainly contains proteoglycan (grape ammonia glycan (GAG)) and fibrin composition, they two all there is nanostructured composition; Research shows that nanostructured support contributes to cell adhesion and propagation, and function is higher than micro-meter scale; This be due to polymer nanofiber can be potential imitation n cell epimatrix structure, chemical composition and mechanical performance, in this case, they instruct behavior and the function of cell as timbering material, until host cell can bear a new natural substrates again. Therefore polymer nanofiber causes broad research at regenerative medicine and field of tissue engineering technology.
Sodium alginate, due to its composition similar to extracellular matrix and premium properties, has huge potential application foreground at regenerative medicine and field of tissue engineering technology; But because sodium alginate is a kind of polyelectrolyte, pure sodium alginate Static Spinning is very difficult; At present, the method that realizes sodium alginate electrostatic spinning generally has following several: (1) adds intensive polar solvent and surfactant, divide flexibility and the degree of entanglement of riding chain and reduce surface tension to strengthen sodium alginate, making sodium alginate have enough entanglement degree to form fiber; (2) blending is to facilitate the electrostatic spinning of sodium alginate with it as carrier polymer to introduce spinnability water-soluble polymer, and this is mainly the high degree of entanglement that has utilized carrier polymer, even if also can form fiber in the situation that sodium alginate exists.
In prior art, the technical scheme of utilizing above-mentioned principle to realize sodium alginate electrospun nanofibers film also has a lot, such as:
The application for a patent for invention " nano fiber scaffold material taking sodium alginate as matrix and preparation method thereof " of publication number CN101011597A, by intensive polar solvent glycerine, and carrier polymer polyethylene glycol oxide or polyvinyl alcohol, prepare the micro/nano fibrous membrane material that sodium alginate and polyethylene glycol oxide or polyvinyl alcohol mass ratio are 6:4-9:1, in this material, the content of sodium alginate and polyethylene glycol oxide or polyvinyl alcohol is 90%-95%, and glycerine content is 5%-10%; , in the time using as timbering material, there is larger security risk in the chemical reagent glycerine and residual more that changed materials'use.
The application for a patent for invention " preparation method of pure sodium alginate nano fiber membrane material " of publication number CN101230150A, taking the mixture of glycerine or glycerine and ethylene glycol as modifier, the mixture of water or water and ethanol is solvent, has made pure sodium alginate nano fiber film using the copper mesh that is immersed in the ethanol water that contains calcium chloride as receiver; Change the sodium alginate nano fiber film purity that method makes higher, but exist process comparatively loaded down with trivial details, the problem that efficiency is lower, and there is equally the problem of chemical agent residue.
The application for a patent for invention " a kind of preparation method of modified sodium alginate electro spinning nano fiber " of publication number CN103046162A, using EDC-HCl as catalyst, sodium alginate is reacted to the sodium alginate that makes modification with octylame, then 2% modification modified sodium alginate solution and 8% PVA solution are mixed and carry out electrostatic spinning and make modified sodium alginate nano fibrous membrane with 2:8 ratio. The nano fibrous membrane that the method makes need not carry out crosslinking Treatment and just have good hydrophobic performance. But exist the problem that sodium alginate content is lower can affect its serviceability.
In a word, technique scheme and other are similarly prepared two problems of method ubiquity of sodium alginate nano fiber film: in (1) preparation process, have the chemical reagent such as modifier, intensive polar solvent to use, on the nano fibrous membrane that makes to make, there is reagent residual, thereby have security risk; (2) do not add in the nano fibrous membrane that chemical reagent and other spinnability mixed with polymers electrostatic spinning make sodium alginate content very low, limited the performance of nano fibrous membrane, restricted its application.
Summary of the invention
The object of the invention is to provide in order to solve the problems of the technologies described above a kind of electrostatic spinning preparation method of high-load sodium alginate nano fiber film; This material is made up of sodium alginate or sodium alginate and polyvinyl alcohol, and wherein the absolute content of sodium alginate is 42.5wt%-100wt%, and average fibre diameter is between 100nm-150nm; Preparation method is simple, and adds without any harmful substance.
The present invention takes following technical scheme for achieving the above object: sodium alginate soln and polyethylene oxide solutions or polyethylene glycol oxide and poly-vinyl alcohol solution are mixed with certain proportion; After mixing, add again the surfactant TX-100 of 0.5wt%-2wt% to mix again; The spinning solution mixing is injected to needle tubing, utilize electrostatic spinning apparatus to make nano fibrous membrane. Nano fibrous membrane again in baking oven high-temperature process 1-3h remove polyethylene glycol oxide and obtain sodium alginate or sodium alginate/polyvinyl alcohol nano film, the average diameter of the nano fibrous membrane of gained is at 100nm-150nm.
Concrete preparation method of the present invention is:
(1) preparation of electrostatic spinning liquid: sodium alginate, polyethylene glycol oxide and (or) polyvinyl alcohol are dissolved in respectively in deionized water and stir acquisition certain density sodium alginate soln, polyethylene oxide solutions and (or) poly-vinyl alcohol solution, and then sodium alginate soln, polyethylene oxide solutions and (or) poly-vinyl alcohol solution are blended into mixed solution with certain mass ratio, and to add mass fraction be that the TX-100 of 0.5wt%-2wt% stirs and discontinuous degassing obtains electrostatic spinning solution;
(2) preparation of composite nano-fiber membrane: electrostatic spinning solution is injected to the electrostatic spinning apparatus needle tubing of (as shown in Figure 1), and regulation voltage is 12-25kV, shower nozzle is 5-22cm to the distance of receiver, flow is 0.2-1.5ml/h. Open device for spinning, can on receiver, collect sodium alginate composite nano-fiber membrane;
(3) high-temperature process: the sodium alginate composite nano-fiber membrane obtaining is placed in vacuum drying oven, adjusts the temperature of baking oven to 90-120 degree, drying 1-3h, can obtain sodium alginate or sodium alginate/polyvinyl alcohol nano film.
The present invention is by mixing sodium alginate with polyethylene glycol oxide and (or) polyvinyl alcohol, under the condition taking water as solvent, realize electrostatic spinning, after electrostatic spinning completes, utilize again the fusing point difference of polyethylene glycol oxide and sodium alginate, polyvinyl alcohol, obtained the higher or even pure sodium alginate nano fiber of sodium alginate content by high-temperature process. Preparation process is simple, environmental protection, and the nano fibrous membrane of preparation has the advantages that fibre diameter is thin, voidage is high, nontoxic.
Beneficial effect of the present invention is: sodium alginate soln is mixed and carries out electrostatic spinning with polyethylene oxide solutions and (or) poly-vinyl alcohol solution, can significantly improve the spinning condition of sodium alginate, under the condition that is solvent at water, just can realize electrostatic spinning, avoid the use of the chemical reagent such as intensive polar solvent, eliminated the security risk that chemical agent residue is brought, TX-100 is a kind of by the nonionic surface active agent of food and drug administration (FDA) certification, be widely used in immunocytochemistry and life science, it can improve the spinning condition of sodium alginate, there is again extremely low cytotoxicity, make the biomedical sectors such as the nano fibrous membrane energy application cell cultivation making, the fusing point of polyethylene glycol oxide is 65 degree left and right, the fusing point of sodium alginate and polyvinyl alcohol is all more than 150 degree, utilize the fusing point difference that polyethylene glycol oxide and sodium alginate and polyvinyl alcohol are larger, sodium alginate composite nano-fiber membrane standby electro-spinning is placed in vacuum drying oven to drying under the condition of 90-120 DEG C can be removed polyethylene glycol oxide and can not have damage to sodium alginate and polyvinyl alcohol, thereby can obtain even pure sodium alginate fiber of a high proportion of sodium alginate fiber, solve the problem of a high proportion of sodium alginate fiber and pure sodium alginate fiber electrostatic difficulty in spinning, and in the nano fibrous membrane obtaining, the average diameter of fiber is thinner, voidage is high, can be applied to wound dressing and field of tissue engineering technology (as timbering material).
Brief description of the drawings
Accompanying drawing 1 is electrostatic spinning apparatus, and accompanying drawing 2, accompanying drawing 3, accompanying drawing 4 respectively corresponding embodiment 1, embodiment 2, embodiment 3 sodium alginate nano fiber films amplify the stereoscan photograph of 8000 times.
Detailed description of the invention
Further illustrate the present invention below in conjunction with embodiment and accompanying drawing thereof;
Embodiment 1
(1) spinning solution preparation: it is the sodium alginate soln of 3wt% that a certain amount of sodium alginate is dissolved in to the preparation quality mark that at room temperature stirs in deionized water, it is the polyethylene oxide solutions of 3wt% that a certain amount of polyethylene glycol oxide is dissolved in to the preparation quality mark that at room temperature stirs in deionized water, and it is the poly-vinyl alcohol solution of 8wt% that a certain amount of poly-vinyl alcohol solution is dissolved in to the preparation quality mark that stirs under 90 DEG C of conditions in deionized water; Then sodium alginate soln, polyethylene oxide solutions and poly-vinyl alcohol solution are mixed with mass ratio 4:4:2, at room temperature stir and obtain homogeneous mixed solution, then be that the TX-100 of 0.5wt% at room temperature stirs and obtains electrostatic spinning solution toward adding mass fraction in homogeneous mixed solution;
(2) preparation of composite nano-fiber membrane: leave standstill 24h under electrostatic spinning solution room temperature prepared by step (1) and remove bubble, afterwards spinning solution injected to the needle tubing of electrostatic spinning apparatus and connect with syringe pump, select No. 21 pins as spinning head, be covered with the rotatable circular disc of aluminium-foil paper as receiver, the distance of spinning head and receiver is 20cm; On syringe needle, apply the high pressure of 16kV, regulating the flow velocity of syringe pump is 0.4ml/h, and the slewing rate of disk receiver is 160r/min, obtains the sodium alginate composite nano-fiber membrane of certain area after spinning a period of time;
(3) high-temperature process: the sodium alginate composite nano-fiber membrane that step (2) is obtained is placed in vacuum drying oven, regulating the temperature in baking oven is 90 DEG C, drying 2h under 90 DEG C of conditions, sodium alginate/polyvinyl alcohol composite nano-line the film that obtains removing polyethylene glycol oxide, its average fibre diameter is 159.6nm.
Embodiment 2
(1) spinning solution preparation: it is the sodium alginate soln of 3wt% that a certain amount of sodium alginate is dissolved in to the preparation quality mark that at room temperature stirs in deionized water, it is the polyethylene oxide solutions of 3wt% that a certain amount of polyethylene glycol oxide is dissolved in to the preparation quality mark that at room temperature stirs in deionized water, and it is the poly-vinyl alcohol solution of 8wt% that a certain amount of poly-vinyl alcohol solution is dissolved in to the preparation quality mark that stirs under 90 degree conditions in deionized water. Then sodium alginate soln, polyethylene oxide solutions and poly-vinyl alcohol solution are mixed with mass ratio 5:4:1, at room temperature stir and obtain homogeneous mixed solution, then be that the TX-100 of 1wt% at room temperature stirs and obtains electrostatic spinning solution toward adding mass fraction in homogeneous mixed solution;
(2) preparation of composite nano-fiber membrane: leave standstill 24h under electrostatic spinning solution room temperature prepared by step (1) and remove bubble, afterwards spinning solution injected to the needle tubing of electrostatic spinning apparatus and connect with syringe pump, select No. 21 pins as spinning head, be covered with the rotatable circular disc of aluminium-foil paper as receiver, the distance of spinning head and receiver is 18cm; On syringe needle, apply the high pressure of 18kV, regulating the flow velocity of syringe pump is 0.8ml/h, and the slewing rate of disk receiver is 170r/min, obtains the sodium alginate composite nano-fiber membrane of certain area after spinning a period of time;
(3) high-temperature process: the sodium alginate composite nano-fiber membrane that step (2) is obtained is placed in vacuum drying oven, regulating the temperature in baking oven is 100 DEG C, drying 1h under 90 DEG C of conditions, sodium alginate/polyvinyl alcohol composite nano-line the film that obtains removing polyethylene glycol oxide, its average fibre diameter is 103.6nm.
Embodiment 3
(1) spinning solution preparation: it is the sodium alginate soln of 3wt% that a certain amount of sodium alginate is dissolved in to the preparation quality mark that at room temperature stirs in deionized water, it is the polyethylene oxide solutions of 3wt% that a certain amount of polyethylene glycol oxide is dissolved in to the preparation quality mark that at room temperature stirs in deionized water. Then sodium alginate soln and polyethylene oxide solutions are mixed with mass ratio 5:5, at room temperature stir and obtain homogeneous mixed solution, then be that the TX-100 of 1.5wt% at room temperature stirs and obtains electrostatic spinning solution toward adding mass fraction in homogeneous mixed solution;
(2) preparation of composite nano-fiber membrane: leave standstill 24h under electrostatic spinning solution room temperature prepared by step (1) and remove bubble, afterwards spinning solution injected to the needle tubing of electrostatic spinning apparatus and connect with syringe pump, select No. 21 pins as spinning head, be covered with the rotatable circular disc of aluminium-foil paper as receiver, the distance of spinning head and receiver is 16cm; On syringe needle, apply the high pressure of 14kV, regulating the flow velocity of syringe pump is 0.5ml/h, and the slewing rate of disk receiver is 175r/min, obtains the sodium alginate composite nano-fiber membrane of certain area after spinning a period of time;
(3) high-temperature process: the sodium alginate composite nano-fiber membrane that step (2) is obtained is placed in vacuum drying oven, regulating the temperature in baking oven is 120 DEG C, drying 1h under 90 DEG C of conditions, the sodium alginate nano wire film that obtains removing polyethylene glycol oxide, its average fibre diameter is 134.5nm.
Claims (3)
1. a high-load sodium alginate nano fiber film and electrostatic spinning preparation method thereof.
2. this material is made up of sodium alginate or sodium alginate and polyvinyl alcohol, and the absolute content of sodium alginate is 42.5wt%-100wt%, and average fibre diameter is between 100nm-150nm;
Preparation method is simple, and adds without any harmful substance;
A kind of high-load sodium alginate nano fiber film according to claim 1 and electrostatic spinning preparation method thereof, is characterized in that the preparation taking water as solvent, and concrete preparation method is:
(1) preparation of electrostatic spinning liquid: sodium alginate, polyethylene glycol oxide and (or) polyvinyl alcohol are dissolved in respectively in deionized water and stir acquisition certain density sodium alginate soln, polyethylene oxide solutions and (or) poly-vinyl alcohol solution, and then molten to sodium alginate soln, polyethylene glycol oxide and (or) poly-vinyl alcohol solution are blended into mixed solution with certain mass ratio, and add the surfactant TX-100 of certain mass mark to stir and discontinuous degassing obtains electrostatic spinning solution;
(2) preparation of composite nano-fiber membrane: electrostatic spinning solution is injected to the needle tubing of electrostatic spinning device, regulation voltage is 12-25kV, shower nozzle is 5-22cm to the distance of receiver, flow is 0.2-1.5ml/h;
Open device for spinning, can on receiver, collect sodium alginate composite nano-fiber membrane;
(3) high-temperature process: the sodium alginate composite nano-fiber membrane obtaining is weaved in vacuum drying oven, adjust the temperature of baking oven to 90-120 DEG C, drying 1-3h, can obtain sodium alginate or sodium alginate/polyvinyl alcohol nano film.
3. the electrostatic spinning preparation method of a kind of high-load sodium alginate nano fiber film according to claim 2, is characterized in that: when high-temperature process, vacuum drying oven temperature is 90-120 DEG C, and the processing time is 1-3h.
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Cited By (12)
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| CN105854069A (en) * | 2016-06-02 | 2016-08-17 | 四川奎星医用高分子制品有限责任公司 | Alginate dressing containing wound-healing promoting medicine and preparing method thereof |
| CN106176045A (en) * | 2016-08-31 | 2016-12-07 | 广州润虹医药科技有限公司 | A kind of alginate dressing of anti and preparation method thereof |
| CN106283269A (en) * | 2016-08-16 | 2017-01-04 | 曹健 | A kind of preparation method of sodium alginate/polyvinyl alcohol nano |
| CN106480608A (en) * | 2016-12-05 | 2017-03-08 | 青岛大学 | A kind of method that employing electrospinning processes prepare coloring sodium alginate nano fiber film |
| CN106729928A (en) * | 2017-01-16 | 2017-05-31 | 武汉理工大学 | A kind of polyvinyl alcohol/sodium alginate/hydroxyapatite composite fiber membrane and preparation method thereof, application |
| CN107385562A (en) * | 2017-07-13 | 2017-11-24 | 青岛大学 | A kind of alginic acid/Nano Silver composite nano fiber and preparation method thereof |
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| CN107794601A (en) * | 2017-09-12 | 2018-03-13 | 浙江理工大学 | For preparing spinning solution and its application of high marine alga content nanofiber |
| CN108283727A (en) * | 2018-03-26 | 2018-07-17 | 广东工业大学 | A kind of nanofiber dressing and preparation method thereof |
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| CN105854069A (en) * | 2016-06-02 | 2016-08-17 | 四川奎星医用高分子制品有限责任公司 | Alginate dressing containing wound-healing promoting medicine and preparing method thereof |
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| CN106176045B (en) * | 2016-08-31 | 2017-07-14 | 广州润虹医药科技有限公司 | A kind of alginate dressing prevented adhesion and preparation method thereof |
| CN106480608B (en) * | 2016-12-05 | 2018-07-06 | 青岛大学 | A kind of method that coloring sodium alginate nano fiber film is prepared using electrospinning processes |
| CN106480608A (en) * | 2016-12-05 | 2017-03-08 | 青岛大学 | A kind of method that employing electrospinning processes prepare coloring sodium alginate nano fiber film |
| CN106729928A (en) * | 2017-01-16 | 2017-05-31 | 武汉理工大学 | A kind of polyvinyl alcohol/sodium alginate/hydroxyapatite composite fiber membrane and preparation method thereof, application |
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| CN107385562A (en) * | 2017-07-13 | 2017-11-24 | 青岛大学 | A kind of alginic acid/Nano Silver composite nano fiber and preparation method thereof |
| CN107794601A (en) * | 2017-09-12 | 2018-03-13 | 浙江理工大学 | For preparing spinning solution and its application of high marine alga content nanofiber |
| CN107794601B (en) * | 2017-09-12 | 2020-01-21 | 浙江理工大学 | Spinning solution for preparing high-algae-content nano fibers and application thereof |
| CN107737366A (en) * | 2017-09-30 | 2018-02-27 | 广东泰宝医疗科技股份有限公司 | A kind of modified sodium alginate electrospinning fibre haemostatic membrane and preparation method thereof |
| CN108283727A (en) * | 2018-03-26 | 2018-07-17 | 广东工业大学 | A kind of nanofiber dressing and preparation method thereof |
| CN112393827A (en) * | 2019-08-12 | 2021-02-23 | 南京理工大学 | Preparation method of biodegradable piezoelectric force sensor |
| CN114318662A (en) * | 2022-01-07 | 2022-04-12 | 蕴能(大连)生物科技有限公司 | Edible sun-proof nanofiber membrane and preparation method thereof |
| CN114853424A (en) * | 2022-05-24 | 2022-08-05 | 绍兴上虞南方普银混凝土有限公司 | Super-retarding durable concrete and preparation process thereof |
| CN114853424B (en) * | 2022-05-24 | 2023-01-10 | 绍兴上虞南方普银混凝土有限公司 | Super-retarding durable concrete and preparation process thereof |
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Application publication date: 20160518 |