CN105200668A - Preparation method of sodium alginate/carbon nanotube hybrid nanofiber membrane - Google Patents

Preparation method of sodium alginate/carbon nanotube hybrid nanofiber membrane Download PDF

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Publication number
CN105200668A
CN105200668A CN201510675556.5A CN201510675556A CN105200668A CN 105200668 A CN105200668 A CN 105200668A CN 201510675556 A CN201510675556 A CN 201510675556A CN 105200668 A CN105200668 A CN 105200668A
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China
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sodium alginate
solution
preparation
carbon nano
carbon nanotube
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CN201510675556.5A
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蔡志江
徐熠
贾建茹
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Abstract

The invention discloses a preparation method of a sodium alginate/carbon nanotube hybrid nanofiber membrane, and belongs to a preparation technology of fiber membrane materials. The method comprises the following steps: firstly, carrying out acidifying treatment on carbon nanotubes until carboxyl groups are formed on the surfaces of the carbon nanotubes, and dispersing the carbon nanotubes into deionized water to prepare a carbon nanotube solution; dissolving the sodium alginate into water to obtain a transparent sodium alginate aqueous solution; and mixing the carbon nanotube solution with the sodium alginate aqueous solution, and carrying out electrostatic spinning, wherein the high-voltage electrostatic adjustment range is 10-30kV; the flow rate of an injection pump is 0.05-0.3mL/h; the receiving distance is 10-20cm. The preparation method disclosed by the invention is simple in process; the obtained sodium alginate/carbon nanotube hybrid nanofiber membrane has the advantage of good adsorption property.

Description

The preparation method of a kind of sodium alginate/carbon nano-tube hybridization nano fibrous membrane
Technical field
The present invention relates to a kind of sodium alginate/CNT (containing single wall and Duo Bi (n=2-20)) carries out spinning film forming preparation method by high-pressure electrostatic, belong to the technology of preparing of fiber film material.
Background technology
Sodium alginate (SA) is natural biological source macromolecular material distributed more widely on the earth, is continuable, not consumable natural material.Sodium alginate has stability, hydrophily, avirulence and biodegradability.Be made up of two kinds of monose, be Isosorbide-5-Nitrae-poly-beta-D-mannuronic acid and α-L-guluronic acid respectively, both connect and compose sodium alginate by straight line.SA is white or pale yellow powder, has tasteless property, odorless, is insoluble to ether, ethanol, Diluted Alcohol liquid, organic solvent, acids (pH value < 3).SA character and its processing technology and prepare its material used and have very large relation.Generally, SA and water form viscous fluid, have high viscosity, when its content is 0.5%, are 1 ~ 100s in shearing -1time, its viscosity is similar to its aqueous solution, relevant with pH value.The Application Areas of sodium alginate widely, mainly contains: medical material, food industry, paper industry, electronic equipment etc.
CNT is a kind of One-dimensional Quantum material with special construction.The structures shape that CNT is special its there is the excellent performance such as mechanics, electromagnetism, calorifics, be widely used in various field.In mechanical property, CNT has excellent tensile strength and elastic modelling quantity, and its elastic modelling quantity is 1TPa, be about the elastic modelling quantity 5 times of steel, tensile strength can reach 50-200GPa, be about 100 times of the tensile strength of steel, and its density is about 1/6 of the density of steel.Therefore, effect CNT being applied to other material as reinforcing material, can reaching toughness reinforcing, strengthen.Along with the maturation of carbon nanotube preparation technology and the continuous reduction of CNT cost, the application study of CNT more and more becomes the emphasis of research.If CNT and sodium alginate are carried out molecule level compound, then carry out electrostatic spinning, be then expected to the fiber film material obtaining having high absorption property.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of sodium alginate/carbon nano-tube hybridization nano fibrous membrane, obtained material has high absorption property in this way.
The present invention is realized by following technical proposals.The preparation method of a kind of sodium alginate/carbon nano-tube hybridization nano fibrous membrane, first CNT is carried out acidification by the method, make its surface with carboxyl, again it is carried out ultrasonic mixing with the sodium alginate be dissolved in water, had the Hybrid nanofibers film of high absorption property by electrostatic spinning preparation, the method is characterized in that comprising following process:
1) preparation of carbon nano-tube solution: single wall or multi-walled carbon nano-tubes are joined by quality HNO 3/ H 2sO 4be in the mixed acid of 1: 1, be mixed with the solution of 0.01 ~ 0.1g/mL, reflux under solution being heated to fluidized state 60-90min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 5 ~ 15mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by molecular weight be at room temperature 1 ~ 80,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 2 ~ 6%, magnetic agitation 6h, obtain transparent sodium alginate aqueous solution;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.05: 1 ~ 0.25: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, high-pressure electrostatic adjustable range 10 ~ 30kV, syringe pump flow velocity 0.05 ~ 0.3mL/h, receiving range 10 ~ 20cm, obtaining diameter is 200 ~ 500nm tunica fibrosa.
Preparation method's process of the present invention is simple, obtain the advantage that sodium alginate/carbon nano-tube hybridization nano fibrous membrane has high adsorption.
Detailed description of the invention
Embodiment 1:
1) preparation of carbon nano-tube solution: HNO 4.0g Single Walled Carbon Nanotube being joined 200ml 3/ H 2sO 4in the mixed acid of (1: 1), be mixed with the solution of 0.02g/mL, reflux under solution being heated to fluidized state 60min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 6.0mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by certain molecular weight be at room temperature 60,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 3.5%, magnetic agitation 6h, the transparent sodium alginate aqueous solution of acquisition;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.05: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, spinning voltage 20kV, syringe pump flow velocity 0.2mL/h, receiving range 20cm, obtaining diameter is 300 ~ 400nm tunica fibrosa.
Embodiment 2:
1) preparation of carbon nano-tube solution: HNO 4.0g Single Walled Carbon Nanotube being joined 100ml 3/ H 2sO 4in the mixed acid of (1: 1), be mixed with the solution of 0.04g/mL, reflux under solution being heated to fluidized state 70min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 8.0mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by certain molecular weight be at room temperature 80,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 2%, magnetic agitation 6h, the transparent sodium alginate aqueous solution of acquisition;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.1: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, spinning voltage 10kV, syringe pump flow velocity 0.3mL/h, receiving range 10cm, obtaining diameter is 400 ~ 500nm tunica fibrosa.
Embodiment 3:
1) preparation of carbon nano-tube solution: HNO 8.0g Single Walled Carbon Nanotube being joined 100ml 3/ H 2sO 4in the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, reflux under solution being heated to fluidized state 90min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 10mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by certain molecular weight be at room temperature 10,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 6%, magnetic agitation 6h, obtain transparent sodium alginate aqueous solution;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.15: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, spinning voltage 30kV, syringe pump flow velocity 0.05mL/h, receiving range 20cm, obtaining diameter is 200 ~ 300nm tunica fibrosa.
Embodiment 4:
1) preparation of carbon nano-tube solution: HNO 8.0g Single Walled Carbon Nanotube being joined 100ml 3/ H 2sO 4in the mixed acid of (1: 1), be mixed with the solution of 0.08g/mL, reflux under solution being heated to fluidized state 90min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 12mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by certain molecular weight be at room temperature 30,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 4.5%, magnetic agitation 6h, obtain transparent sodium alginate aqueous solution;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.20: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, spinning voltage 20kV, syringe pump flow velocity 0.1mL/h, receiving range 15cm, obtaining diameter is 350 ~ 450nm tunica fibrosa.

Claims (1)

1. the preparation method of sodium alginate/carbon nano-tube hybridization nano fibrous membrane, first CNT is carried out acidification by the method, make its surface with carboxyl, again it is carried out ultrasonic mixing with the sodium alginate be dissolved in water, had the Hybrid nanofibers film of high absorption property by electrostatic spinning preparation, the method is characterized in that comprising following process:
1) carbon nano-tube solution preparation: single wall or multi-walled carbon nano-tubes are joined by quality HNO 3/ H 2sO 4be in the mixed acid of 1: 1, be mixed with the solution of 0.01 ~ 0.1g/mL, reflux under solution being heated to fluidized state 60-90min, deionized water is spent to faintly acid after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried carbon nanotube dispersed in deionized water, it is 5 ~ 15mg/mL carbon nano-tube solution that ultrasonic disperse obtains concentration;
2) preparation of sodium alginate soln: by molecular weight be at room temperature 1 ~ 80,000 sodium alginate be dissolved in the water, be mixed with the solution that mass fraction is 2 ~ 6%, magnetic agitation 6h, obtain transparent sodium alginate aqueous solution;
3) preparation of composite solution: by step 1) carbon nano-tube solution and the step 2 that obtain) sodium alginate aqueous solution that obtains mixes according to the mass ratio 0.05: 1 ~ 0.25: 1 of solute, and at room temperature ultrasonic disperse 2h;
4) preparation of Hybrid nanofibers film: by step 3) composite solution that obtains joins in syringe, and be fixed on micro-injection pump, the aluminium foil placing vertical ground connection apart from syringe needle a distance receives, high-pressure electrostatic adjustable range 10 ~ 30kV, syringe pump flow velocity 0.05 ~ 0.3mL/h, receiving range 10 ~ 20cm, obtaining diameter is 200 ~ 500nm tunica fibrosa.
CN201510675556.5A 2015-10-19 2015-10-19 Preparation method of sodium alginate/carbon nanotube hybrid nanofiber membrane Pending CN105200668A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106498625A (en) * 2016-10-24 2017-03-15 天津工业大学 A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof
CN107799200A (en) * 2017-10-11 2018-03-13 哈尔滨工程大学 A kind of process of preparing of sodium alginate/multi-walled carbon nanotube electrode film
CN115341339A (en) * 2022-08-25 2022-11-15 武汉大学 Silk fibroin composite fiber membrane for detecting and analyzing perfluorinated polyfluoro compounds and method

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106498625A (en) * 2016-10-24 2017-03-15 天津工业大学 A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof
CN106498625B (en) * 2016-10-24 2018-09-14 天津工业大学 A kind of poly butyric ester/carbon nano tube composite nanofiber membrane and preparation method thereof
CN107799200A (en) * 2017-10-11 2018-03-13 哈尔滨工程大学 A kind of process of preparing of sodium alginate/multi-walled carbon nanotube electrode film
CN107799200B (en) * 2017-10-11 2020-06-16 哈尔滨工程大学 Preparation process method of sodium alginate/multi-walled carbon nanotube electrode film
CN115341339A (en) * 2022-08-25 2022-11-15 武汉大学 Silk fibroin composite fiber membrane for detecting and analyzing perfluorinated polyfluoro compounds and method
CN115341339B (en) * 2022-08-25 2024-03-22 武汉大学 Silk fibroin composite fiber film and method for detecting and analyzing perfluoro-type compounds

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Application publication date: 20151230