CN105457094A - Calcium chloride cross-linked sodium alginate nanometer fiber scaffold material and preparation method thereof - Google Patents
Calcium chloride cross-linked sodium alginate nanometer fiber scaffold material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a calcium chloride cross-linked sodium alginate nanometer fiber scaffold material and a preparation method thereof. The material comprises sodium alginate and polyvinyl alcohol according to a ratio of the sodium alginate to the polyvinyl alcohol of 5:5-9:1, wherein the average diameter of the nanometer fiber membrane fibers is 50-200 nm, the breaking strength is greater than 1 MPa, and the water absorption rate is greater than 70%. According to the present invention, the calcium chloride is used to cross-link the sodium alginate solution so as to improve the spinnability of the sodium alginate, the isopropyl alcohol content in the electrostatic spinning liquid is controlled at less than or equal to 5 wt% through assisted uses of a surfactant TX-100 and a co-solvent ethanol, the isopropyl alcohol can be removed during the final nanometer fiber membrane cross-linking treatment process, and the finally obtained sodium alginate nanometer fiber scaffold material can completely meet the use requirements of tissue engineering.
Description
Technical field
The invention belongs to polymeric material field, relate to calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination and preparation method thereof specifically.
Background technology
Sodium alginate is a kind of natural polysaccharide mainly coming from algae, forms primarily of Isosorbide-5-Nitrae-beta-D-mannuronic acid (M unit) and α-L-guluronic acid (G unit), similar to the protein-polysaccharide composition in human body cell epimatrix.Sodium alginate also has that source is wide, good biocompatibility, have the good characteristics such as controlled biological degradability and nonhazardous and can not cause antigen-reactive.These characteristics make it have huge application potential in field of tissue engineering technology.At present about the applied research of sodium alginate in organizational project more be the porous sodium alginate frozen film prepared by freeze-drying.But the film of perforated membrane prepared by freeze-drying and hole aperture size many in micron level, and the main component proteoglycan (Fructus Vitis viniferae ammonia polysaccharide (GAG)) of natural extracellular matrix in tissue and fibrin all have nanostructured composition.Research shows that nanostructured support contributes to cell adhesion and propagation, and function is higher than micro-meter scale.The main method preparing nanofiber is at present electrostatic spinning.But because sodium alginate is a kind of polyelectrolyte, pure sodium alginate Static Spinning is very difficult.At present, want to realize sodium alginate electrostatic spinning, in sodium alginate solution, only add intensive polar solvent and surfactant strengthen the motility of sodium alginate strand and degree of entanglement and reduce surface tension, make sodium alginate have enough entanglement degree to form fiber, or the carrier polymer that introducing is easily spun utilize the high degree of entanglement of carrier polymer to realize the spinning of sodium alginate.But conventional at present intensive polar solvent such as dimethylformamide and dimethyl trident maple etc. all have toxicity, in the nano fibrous membrane of preparation, the residual cultivation that can affect cell is had after volume uses, and due to the water-soluble nature of sodium alginate, sodium alginate nano fiber film has the problem of poor water resistance.
Summary of the invention
The object of the invention is to provide calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination and preparation method thereof to solve the problems of the technologies described above.This material is made up of sodium alginate and polyvinyl alcohol, and wherein the ratio of sodium alginate and polyvinyl alcohol is 5:5-9:1, and the average diameter of nanofiber membrane fiber is between 50nm-200nm, and fracture strength is greater than 1MPa, and water absorption rate is greater than 70%.
The present invention takes following technical scheme for achieving the above object: prepare the calcium cross-linked sodium alginate soln of a certain amount of chlorination and mix homogeneously with certain proportion with poly-vinyl alcohol solution.The surfactant TX-100 adding 0.5wt%-2wt% after mix homogeneously again carries out mix homogeneously again.The spinning liquid of mix homogeneously is injected needle tubing, utilizes electrostatic spinning apparatus to obtain nano fibrous membrane.Nano fibrous membrane is cross-linked 2h further again in the alcoholic solution containing 0.5wt%-5wt% calcium chloride, puts to dry in an oven both to obtain sodium alginate nano fiber timbering material after clear water cyclic washing again, and the average diameter of the nano fibrous membrane of gained is at 50nm-200nm.
Concrete preparation method of the present invention is:
(1) calcium chloride crossslinked sodium alginate solution: sodium alginate being dissolved in preparation quality mark in deionized water is the sodium alginate soln of 3wt%; In the mixed solution of calcium chloride is water-soluble, ethanol and isopropyl alcohol (mass ratio of water, ethanol and isopropyl alcohol is 0:85:15-75:15:10), mixed solution to be instilled mass fraction be in the sodium alginate soln of 3wt% again until the content of calcium chloride is the 1%-3% of sodium alginate quality and stir process 2h, and now the mass fraction of sodium alginate soln is 2wt%.
(2) preparation of poly-vinyl alcohol solution: a certain amount of polyvinyl alcohol is dissolved in deionized water stir under the condition of 90 DEG C 4h obtain mass fraction be the poly-vinyl alcohol solution of 8wt%.
(3) preparation of electrostatic spinning liquid: the calcium cross-linked sodium alginate soln of chlorination of 2wt% step (1) obtained and the poly-vinyl alcohol solution of 8wt% are blended into mixed solution with mass ratio 5:5-9:1, and add mass fraction and be that the TX-100 of 0.5wt%-2wt% stirs and discontinuous degassing obtains electrostatic spinning solution.
(4) preparation of nano fibrous membrane: needle tubing electrostatic spinning solution being injected electrostatic spinning apparatus (as shown in Figure 1), regulation voltage is 12-25kV, and shower nozzle is 5-20cm to the distance of receptor, and flow is 0.1-1.5ml/h.Open device for spinning, sodium alginate nano fiber film can be collected on the receiver.
(5) crosslinking Treatment: immersed by the sodium alginate nano fiber film obtained in the alcoholic solution containing 0.5wt%-5wt% calcium chloride and carry out further crosslinking Treatment 2h, takes out cyclic washing in deionized water and puts for 3-4 time again and to dry to baking oven and to obtain sodium alginate nano-bracket material.
The advantage that the present invention prepares sodium alginate nano fiber film is: first by sodium alginate soln is added calcium chloride carry out crosslinking Treatment reduce sodium alginate regularity, reduce degree of crystallinity and add viscosity, which not only improves the spinnability of sodium alginate, the use amount of polar solvent can also be reduced, the security risk that polar solvent brings can be reduced, isopropyl alcohol is a kind of polyol, a kind of than dimethylformamide and the more efficient polar solvent of dimethyl trident maple, this just can reduce the use amount of organic solvent under the prerequisite improving child's acid sodium Static Spinning performance, the present invention is also by introducing the content not too large change of ratio isopropyl alcohol to 9:1 of ethanol and surfactant TX-100 raising sodium alginate, in the electrostatic spinning liquid be finally made into, the content of isopropyl alcohol is lower than 5wt%, and finally can be removed in the crosslinking Treatment of nano fibrous membrane, the sodium alginate nano fiber obtained is made to have high-performance, environmental protection, nontoxic feature, timbering material can be used as.
Accompanying drawing explanation
Accompanying drawing 1 is electrostatic spinning apparatus, accompanying drawing 2 is sodium alginate/polyvinyl alcohol (5:5) nano fibrous membrane SEM (8000 times) picture of embodiment 1 correspondence, accompanying drawing 3 is sodium alginate/polyvinyl alcohol (6:4) nano fibrous membrane SEM (8000 times) picture of embodiment 2 correspondence, and accompanying drawing 4 is sodium alginate/polyvinyl alcohol (7:3) nano fibrous membrane SEM (8000 times) picture of embodiment 3 correspondence.
detailed description of the invention
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing thereof.
embodiment 1
(1) calcium chloride crossslinked sodium alginate solution: sodium alginate being dissolved in preparation quality mark in deionized water is the sodium alginate soln of 3wt%; In the mixed solution of calcium chloride is water-soluble, ethanol and isopropyl alcohol (mass ratio of water, ethanol and isopropyl alcohol is 75:15:10), mixed solution to be instilled mass fraction be in the sodium alginate soln of 3wt% again until the content of calcium chloride be sodium alginate quality 1% and stir process 2h, and now the mass fraction of sodium alginate soln is 2wt%.
(2) preparation of poly-vinyl alcohol solution: a certain amount of polyvinyl alcohol is dissolved in deionized water stir under the condition of 90 DEG C 4h obtain mass fraction be the poly-vinyl alcohol solution of 8wt%.
(3) preparation of electrostatic spinning liquid: the calcium cross-linked sodium alginate soln of chlorination of 2wt% step (1) obtained and the poly-vinyl alcohol solution of 8wt% are blended into mixed solution with mass ratio 5:5, and add mass fraction and be that the TX-100 of 0.5wt% stirs and discontinuous degassing obtains electrostatic spinning solution.
(4) preparation of nano fibrous membrane: needle tubing electrostatic spinning solution being injected electrostatic spinning apparatus (as shown in Figure 1), regulation voltage is 16kV, and shower nozzle is 14cm to the distance of receptor, and flow is 0.4ml/h.Open device for spinning, sodium alginate nano fiber film can be collected on the receiver.
(5) crosslinking Treatment: immersed by the sodium alginate nano fiber film obtained in the alcoholic solution containing 4wt% calcium chloride and carry out further crosslinking Treatment 2h, takes out cyclic washing in deionized water and puts for 3-4 time again and to dry to baking oven and to obtain sodium alginate nano-bracket material.The average diameter recording nano fibrous membrane is 128.6nm, and water absorption rate is 71.98%, and fracture strength is 1.47MPa.
embodiment 2
(1) calcium chloride crossslinked sodium alginate solution: sodium alginate being dissolved in preparation quality mark in deionized water is the sodium alginate soln of 3wt%; In the mixed solution of calcium chloride is water-soluble, ethanol and isopropyl alcohol (mass ratio of water, ethanol and isopropyl alcohol is 55:25:10), mixed solution to be instilled mass fraction be in the sodium alginate soln of 3wt% again until the content of calcium chloride be sodium alginate quality 2% and stir process 2h, and now the mass fraction of sodium alginate soln is 2wt%.
(2) preparation of poly-vinyl alcohol solution: a certain amount of polyvinyl alcohol is dissolved in deionized water stir under the condition of 90 DEG C 4h obtain mass fraction be the poly-vinyl alcohol solution of 8wt%.
(3) preparation of electrostatic spinning liquid: the calcium cross-linked sodium alginate soln of chlorination of 2wt% step (1) obtained and the poly-vinyl alcohol solution of 8wt% are blended into mixed solution with mass ratio 6:4, and add mass fraction and be that the TX-100 of 1wt% stirs and discontinuous degassing obtains electrostatic spinning solution.
(4) preparation of nano fibrous membrane: needle tubing electrostatic spinning solution being injected electrostatic spinning apparatus (as shown in Figure 1), regulation voltage is 18kV, and shower nozzle is 16cm to the distance of receptor, and flow is 0.6ml/h.Open device for spinning, sodium alginate nano fiber film can be collected on the receiver.
(5) crosslinking Treatment: immersed by the sodium alginate nano fiber film obtained in the alcoholic solution containing 4wt% calcium chloride and carry out further crosslinking Treatment 2h, takes out cyclic washing in deionized water and puts for 3-4 time again and to dry to baking oven and to obtain sodium alginate nano-bracket material.The average diameter recording nano fibrous membrane is 138.2nm, and water absorption rate is 81.88%, and fracture strength is 1.29MPa.
embodiment 3
(1) calcium chloride crossslinked sodium alginate solution: sodium alginate being dissolved in preparation quality mark in deionized water is the sodium alginate soln of 3wt%; In the mixed solution of calcium chloride is water-soluble, ethanol and isopropyl alcohol (mass ratio of water, ethanol and isopropyl alcohol is 50:35:15), mixed solution to be instilled mass fraction be in the sodium alginate soln of 3wt% again until the content of calcium chloride be sodium alginate quality 2% and stir process 2h, and now the mass fraction of sodium alginate soln is 2wt%.
(2) preparation of poly-vinyl alcohol solution: a certain amount of polyvinyl alcohol is dissolved in deionized water stir under the condition of 90 DEG C 4h obtain mass fraction be the poly-vinyl alcohol solution of 8wt%.
(3) preparation of electrostatic spinning liquid: the calcium cross-linked sodium alginate soln of chlorination of 2wt% step (1) obtained and the poly-vinyl alcohol solution of 8wt% are blended into mixed solution with mass ratio 7:3, and add mass fraction and be that the TX-100 of 1wt% stirs and discontinuous degassing obtains electrostatic spinning solution.
(4) preparation of nano fibrous membrane: needle tubing electrostatic spinning solution being injected electrostatic spinning apparatus (as shown in Figure 1), regulation voltage is 18kV, and shower nozzle is 14cm to the distance of receptor, and flow is 0.2ml/h.Open device for spinning, sodium alginate nano fiber film can be collected on the receiver.
(5) crosslinking Treatment: immersed by the sodium alginate nano fiber film obtained in the alcoholic solution containing 4wt% calcium chloride and carry out further crosslinking Treatment 2h, takes out cyclic washing in deionized water and puts for 3-4 time again and to dry to baking oven and to obtain sodium alginate nano-bracket material.The average diameter recording nano fibrous membrane is 151.3nm, and water absorption rate is 87.96%, and fracture strength is 1.21MPa.
Can find out that sodium alginate nano fiber film water absorption rate prepared by this method is all greater than 70%, fracture strength is greater than 1MPa, and the absolute content of sodium alginate is between 20%-69.2%, is applicable to tissue timbering material completely in conjunction with the embodiments.
Claims (5)
1. calcium cross-linked sodium alginate nano fiber timbering material of chlorination and preparation method thereof; This material is made up of sodium alginate and polyvinyl alcohol, and wherein the ratio of sodium alginate and polyvinyl alcohol is 5:5-9:1, and the average diameter of nanofiber membrane fiber is between 50nm-200nm, and fracture strength is greater than 1MPa, and water absorption rate is greater than 70%.
2. calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination according to claim 1 and preparation method thereof, it is characterized in that using calcium chloride to carry out twice is cross-linked, concrete preparation method is:
(1) calcium chloride crossslinked sodium alginate solution: sodium alginate being dissolved in preparation quality mark in deionized water is the sodium alginate soln of 3wt%; In the mixed solution of calcium chloride is water-soluble, ethanol and isopropyl alcohol (mass ratio of water, ethanol and isopropyl alcohol is 0:85:15-75:15:10), mixed solution to be instilled mass fraction be in the sodium alginate soln of 3wt% again until the content of calcium chloride is the 1%-3% of sodium alginate quality and stir process 2h, and now the mass fraction of sodium alginate soln is 2wt%;
(2) preparation of poly-vinyl alcohol solution: a certain amount of polyvinyl alcohol is dissolved in deionized water stir under the condition of 90 DEG C 4h obtain mass fraction be the poly-vinyl alcohol solution of 8wt%;
(3) preparation of electrostatic spinning liquid: the calcium cross-linked sodium alginate soln of chlorination of 2wt% step (1) obtained and the poly-vinyl alcohol solution of 8wt% are blended into mixed solution with mass ratio 5:5-9:1, and add mass fraction and be that the TX-100 of 0.5wt%-2wt% stirs and discontinuous degassing obtains electrostatic spinning solution;
(4) preparation of nano fibrous membrane: needle tubing electrostatic spinning solution being injected electrostatic spinning apparatus (as shown in Figure 1), regulation voltage is 12-25kV, and shower nozzle is 5-20cm to the distance of receptor, and flow is 0.1-1.5ml/h;
Open device for spinning, sodium alginate nano fiber film can be collected on the receiver;
(5) crosslinking Treatment: immersed by the sodium alginate nano fiber film obtained in the alcoholic solution containing 0.5wt%-5wt% calcium chloride and carry out further crosslinking Treatment 2h, takes out cyclic washing in deionized water and puts for 3-4 time again and to dry to baking oven and to obtain sodium alginate nano-bracket material.
3. calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination according to claim 2 and preparation method thereof, it is characterized in that: in the process of calcium chloride crossslinked sodium alginate solution, first prepare the sodium alginate soln of 3wt%, then to drip calcium chloride solution (solvent is its mass ratio of water, ethanol and isopropyl alcohol is 0:85:15-75:15:10) to the final content of sodium alginate be wherein 2wt%.
4. calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination according to claim 2 and preparation method thereof, it is characterized in that: in the process of calcium chloride crossslinked sodium alginate solution, the final content of calcium chloride is the 1%-3% of sodium alginate quality.
5. calcium cross-linked sodium alginate nano fiber timbering material of a kind of chlorination according to claim 2 and preparation method thereof, it is characterized in that: in the electrostatic spinning liquid be finally mixed with, the content of isopropyl alcohol is lower than 5%, and it finally can be removed in the crosslinking Treatment of nano fibrous membrane.
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Cited By (12)
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| CN106109447A (en) * | 2016-07-28 | 2016-11-16 | 温州眼视光发展有限公司 | A kind of preparation method and applications of growth factor-loaded sodium alginate/composite membrane of polyvinyl alcohol with levofloxacin |
| CN106283269A (en) * | 2016-08-16 | 2017-01-04 | 曹健 | A kind of preparation method of sodium alginate/polyvinyl alcohol nano |
| CN107281539A (en) * | 2017-06-05 | 2017-10-24 | 江西省科学院应用化学研究所 | A kind of preparation method of soluble paper-like alginates compound hemostatic film |
| CN107675359A (en) * | 2017-09-25 | 2018-02-09 | 湖南农业大学 | A kind of Propiram/sodium alginate composite fiber film and its preparation method and application |
| CN108795921A (en) * | 2017-04-28 | 2018-11-13 | 南京理工大学 | A kind of preparation method of calcium alginate multiphase microcarrier |
| CN109735960A (en) * | 2019-01-29 | 2019-05-10 | 江苏中石纤维股份有限公司 | A kind of preparation method of alginate fiber |
| CN109944072A (en) * | 2019-03-18 | 2019-06-28 | 温州优巴信息技术有限公司 | A kind of sodium alginate nonwoven cloth material and preparation method thereof containing double pyrene nano particles |
| CN111020745A (en) * | 2019-12-31 | 2020-04-17 | 泰州市榕兴医疗用品股份有限公司 | Preparation method of sodium alginate and chitosan composite nanofiber |
| CN112251919A (en) * | 2020-09-30 | 2021-01-22 | 武汉纺织大学 | Unidirectional moisture-transmitting fabric and preparation method thereof |
| CN113463222A (en) * | 2021-05-31 | 2021-10-01 | 南京林业大学 | High-orientation-degree alginic acid fiber and preparation method thereof |
| CN114108319A (en) * | 2021-12-03 | 2022-03-01 | 山西大学 | Preparation method and application of Shewanella embedded gel fiber |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106109447A (en) * | 2016-07-28 | 2016-11-16 | 温州眼视光发展有限公司 | A kind of preparation method and applications of growth factor-loaded sodium alginate/composite membrane of polyvinyl alcohol with levofloxacin |
| CN106283269A (en) * | 2016-08-16 | 2017-01-04 | 曹健 | A kind of preparation method of sodium alginate/polyvinyl alcohol nano |
| CN108795921A (en) * | 2017-04-28 | 2018-11-13 | 南京理工大学 | A kind of preparation method of calcium alginate multiphase microcarrier |
| CN107281539A (en) * | 2017-06-05 | 2017-10-24 | 江西省科学院应用化学研究所 | A kind of preparation method of soluble paper-like alginates compound hemostatic film |
| CN107675359B (en) * | 2017-09-25 | 2019-11-26 | 湖南农业大学 | A kind of Propiram/sodium alginate composite fiber film and its preparation method and application |
| CN107675359A (en) * | 2017-09-25 | 2018-02-09 | 湖南农业大学 | A kind of Propiram/sodium alginate composite fiber film and its preparation method and application |
| CN109735960A (en) * | 2019-01-29 | 2019-05-10 | 江苏中石纤维股份有限公司 | A kind of preparation method of alginate fiber |
| CN109944072A (en) * | 2019-03-18 | 2019-06-28 | 温州优巴信息技术有限公司 | A kind of sodium alginate nonwoven cloth material and preparation method thereof containing double pyrene nano particles |
| CN111020745A (en) * | 2019-12-31 | 2020-04-17 | 泰州市榕兴医疗用品股份有限公司 | Preparation method of sodium alginate and chitosan composite nanofiber |
| CN112251919A (en) * | 2020-09-30 | 2021-01-22 | 武汉纺织大学 | Unidirectional moisture-transmitting fabric and preparation method thereof |
| CN113463222A (en) * | 2021-05-31 | 2021-10-01 | 南京林业大学 | High-orientation-degree alginic acid fiber and preparation method thereof |
| WO2022252955A1 (en) * | 2021-05-31 | 2022-12-08 | 南京林业大学 | Hydroxylated alginate fiber and preparation method therefor |
| CN114108319A (en) * | 2021-12-03 | 2022-03-01 | 山西大学 | Preparation method and application of Shewanella embedded gel fiber |
| CN114108319B (en) * | 2021-12-03 | 2023-09-22 | 山西大学 | Preparation method and application of gel fiber embedded with Shewanella |
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