CN103898676A - Cellulose acetate/ titanium dioxide composite nanofiber adsorption film and preparation method thereof - Google Patents
Cellulose acetate/ titanium dioxide composite nanofiber adsorption film and preparation method thereof Download PDFInfo
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- CN103898676A CN103898676A CN201410108439.6A CN201410108439A CN103898676A CN 103898676 A CN103898676 A CN 103898676A CN 201410108439 A CN201410108439 A CN 201410108439A CN 103898676 A CN103898676 A CN 103898676A
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Abstract
The invention discloses a cellulose acetate/ titanium dioxide composite nanofiber adsorption film and a preparation method of the cellulose acetate/ titanium dioxide composite nanofiber adsorption film, and belongs to a preparation technology of nanometer materials. The method includes the following processes that firstly, alcoholization processing is conducted on titanium dioxide, the surface of titanium dioxide is made to be provided with hydroxyl (TiO2-OH), and a titanium dioxide solution is prepared by dispersing titanium dioxide in deionized water; cellulose acetate is dissolved into a solvent, and a transparent cellulose acetate solution is obtained; the titanium dioxide solution and the cellulose acetate solution are mixed, and electrostatic spinning is conducted, wherein the high-voltage static adjusting range is from 16 kV to 30 kV, the flow speed of an injection pump ranges from 0.05 mL/h to 0.3 mL/h, and the receiving distance ranges from 10 cm to 20 cm. The preparation method is simple in process, and the prepared cellulose acetate/ titanium dioxide composite nanofiber adsorption film has the advantage of being high in heavy metal ion adsorption capacity and adsorption rate.
Description
Technical field
The present invention relates to a kind of cellulose acetate/titanium dioxide is spun to nano fibrous membrane preparation method by high-pressure electrostatic, belong to the technology of preparing of nano material.
Background technology
Along with expanding economy, the discharge of plurality of heavy metal waste water, more and more serious on the impact of environmental and human health impacts, and also heavy metal can not natural degradation in environment, can build up, therefore research and develop safe, efficient, free of contamination heavy metal absorbent and just seem particularly important.Nano material because particle diameter is little, large, the surface of specific area exist great amount of hydroxy group can with CATION bonding, metal ion is shown to stronger adsorption capacity, be a kind of sorbing material that has huge applications prospect.Cellulose acetate (CA) is cellulosic derivative, has the organic solvent of being soluble in, abundant raw material, the feature such as cheap, biodegradable.The film of being prepared by cellulose acetate has that selective height, permeable amount are large, preparation technology simple and the advantage such as excellent optical characteristics, is therefore widely used in the fields such as filtration, absorption.But this porous cellulose acetate membrane also exists adsorption efficiency low, the shortcoming of poor selectivity.Electrostatic spinning is a kind of process technology that makes charged polymer solution or melt jet in electrostatic field prepare polymer superfine fibre, average diameter scope generally at several microns between tens nanometers, it is considered to one of most effectual way of preparing nano grade polymer continuous filament yarn.Fibre diameter that electrostatic spinning technique makes is little, specific area is large, porosity is high, is particularly suitable for being applied in the adsorbing separation field of heavy metal ion.But cellulose acetate nanofiber prepared by electrostatic spinning, mechanical strength is lower, cannot directly apply.Titanium dioxide (TiO
2) thering is the Ti-O key that polarity is larger, the water of adsorption dissociates because of polarization, easily forms hydroxyl, and this surface hydroxyl can improve TiO
2as the performance of adsorbent and various carriers, for surface modification is provided convenience.Meanwhile, adopt TiO
2dichlorodiphenyl Acetate is cellulose nano-fibrous carries out modification, can improve the mechanical strength of cellulose acetate nanofiber, the cellulose acetate/TiO making
2composite nano-fiber membrane mechanical strength is higher, can be directly used in the heavy metal ion in absorption waste water, thereby have broad application prospects.
Summary of the invention
The object of this invention is to provide a kind of preparation method of cellulose acetate/titanium dioxide composite nano fiber adsorbed film, make composite nano fiber adsorbed film with the method and there is higher heavy metal ion adsorbed capacity and the rate of adsorption.
The present invention is realized by following technical proposals.A preparation method for cellulose acetate/titanium dioxide composite nano fiber adsorbed film, first the method refines titanium dioxide processing, makes its surface with hydroxyl (TiO
2-OH), then it is carried out to ultrasonic mixing with the cellulose acetate being dissolved in solvent, prepare the composite nano-fiber membrane with higher heavy metal ion adsorbed capacity and the rate of adsorption by electrostatic spinning, the method is characterized in that comprising following process:
1) titania solution preparation: it is in the ethanol/water of 1: 1 that titanium dioxide nano-particle is joined to quality, be mixed with the solution of 0.01～0.1g/L, by the solution 60-90min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 5～15g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate solution preparation: be at room temperature that 10～500,000 cellulose acetate is dissolved in solvent by molecular weight, be mixed with the solution that volume mass mark (g/L) is 3～15%, magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and step 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute for 0.01: 1～0.15: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 16～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm, obtaining diameter is 220～400nm tunica fibrosa.
Preparation method's process of the present invention is simple, and cellulose acetate/titanium dioxide composite nano fiber adsorbed film that obtains has higher heavy metal ion adsorbed capacity and the rate of adsorption.
Detailed description of the invention
Embodiment 1:
1) titania solution preparation: it is in the liquid in the ethanol/water of 1: 1 that 0.01g titanium dioxide nano-particle is joined to 1L quality, be mixed with the solution of 0.01g/L, by the solution 60min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 5g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate liquid preparation: the cellulose acetate that is at room temperature 100,000 by molecular weight is dissolved in acetone, is mixed with the solution that volume mass mark (g/L) is 15%, and magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and step 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute at 0.15: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 30kV, syringe pump flow velocity 0.05mL/h, receiving range 20cm, obtaining diameter is 220～250nm tunica fibrosa.
Embodiment 2:
1) titania solution preparation: it is in the liquid in the ethanol/water of 1: 1 that 0.04g titanium dioxide nano-particle is joined to 1L quality, be mixed with the solution of 0.04g/L, by the solution 70min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 8g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate liquid preparation: the cellulose acetate that is at room temperature 200,000 by molecular weight is dissolved in chloroform, is mixed with the solution that volume mass mark (g/L) is 10%, and magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and step 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute at 0.1: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 25kV, syringe pump flow velocity 0.1mL/h, receiving range 15cm, obtaining diameter is 280～300nm tunica fibrosa.
Embodiment 3:
1) titania solution preparation: it is in the liquid in the ethanol/water of 1: 1 that 0.08g titanium dioxide nano-particle is joined to 1L quality, be mixed with the solution of 0.08g/L, by the solution 80min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 10g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate liquid preparation: the cellulose acetate that is at room temperature 300,000 by molecular weight is dissolved in dimethylacetylamide, is mixed with the solution that volume mass mark (g/L) is 8%, and magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and step 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute at 0.05: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 20kV, syringe pump flow velocity 0.2mL/h, receiving range 20cm, obtaining diameter is 300～330nm tunica fibrosa.
Embodiment 4:
1) titania solution preparation: it is in the liquid in the ethanol/water of 1: 1 that 0.1g titanium dioxide nano-particle is joined to 1L quality, be mixed with the solution of 0.1g/L, by the solution 90min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 15g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate liquid preparation: the cellulose acetate that is at room temperature 500,000 by molecular weight is dissolved in trifluoroacetic acid, is mixed with the solution that volume mass mark (g/L) is 3%, and magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and the step mule 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute at 0.01: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 16kV, syringe pump flow velocity 0.3mL/h, receiving range 10cm, obtaining diameter is 350～400nm tunica fibrosa.
Claims (3)
1. a preparation method for cellulose acetate/titanium dioxide composite nano fiber adsorbed film, first the method refines titanium dioxide processing, makes its surface with hydroxyl (TiO
2-OH), then it is carried out to ultrasonic mixing with the cellulose acetate being dissolved in solvent, prepare the composite nano-fiber membrane with higher heavy metal ion adsorbed capacity and the rate of adsorption by electrostatic spinning, the method is characterized in that comprising following process:
1) titania solution preparation: it is in the ethanol/water of 1: 1 that titanium dioxide nano-particle is joined to quality, be mixed with the solution of 0.01～0.1g/L, by the solution 60-90min that is heated to reflux under fluidized state, extremely neutral with deionized water washing after filtration, vacuumize 24h at 60 DEG C, get a certain amount of dried titanium dioxide nano-particle and be scattered in deionized water, it is 5～15g/L titania solution that ultrasonic dispersion makes concentration;
2) cellulose acetate solution preparation: be at room temperature that 10～500,000 cellulose acetate is dissolved in solvent by molecular weight, be mixed with the solution that volume mass mark (g/L) is 3～15%, magnetic agitation 6h, obtains transparent solution;
3) composite solution preparation: by step 1) titania solution and step 2 that obtain) cellulose acetate solution of acquisition mixes according to the mass ratio of solute for 0.01: 1～0.15: 1, and at ultrasonic dispersion 2h at room temperature;
4) system of composite nano-fiber membrane: by step 3) obtain composite solution join in syringe, and be fixed on micro-injection pump, the aluminium foil of placing vertical ground connection according to syringe needle a distance receives, high-pressure electrostatic adjustable range 16～30kV, syringe pump flow velocity 0.05～0.3mL/h, receiving range 10～20cm, obtaining diameter is 220～400nm tunica fibrosa.
2. the preparation method of cellulose acetate/titanium dioxide composite nano fiber adsorbed film according to claim 1, is characterized in that described solvent is chloroform, dimethylacetylamide, trifluoroacetic acid or acetone.
3. cellulose acetate/titanium dioxide composite nano fiber adsorbed film of preparing according to claim 1, is characterized in that: described base material is cellulose acetate and titanium dioxide, this adsorption film material has higher heavy metal ion adsorbed capacity and the rate of adsorption.
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| CN105220361A (en) * | 2015-11-04 | 2016-01-06 | 苏州大学 | The preparation method of a kind of Tea Polyphenols/cellulose acetate nano fibrous membrane |
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| CN110396770A (en) * | 2019-07-24 | 2019-11-01 | 常州大学 | A kind of molten spray formula thermoset forming Static Spinning composite membrane and its preparation method and application |
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