CN104928849A - Method for manufacturing cellulose base heat-resisting nano-composite fiber membrane in electrostatic spinning mode - Google Patents
Method for manufacturing cellulose base heat-resisting nano-composite fiber membrane in electrostatic spinning mode Download PDFInfo
- Publication number
- CN104928849A CN104928849A CN201510415614.0A CN201510415614A CN104928849A CN 104928849 A CN104928849 A CN 104928849A CN 201510415614 A CN201510415614 A CN 201510415614A CN 104928849 A CN104928849 A CN 104928849A
- Authority
- CN
- China
- Prior art keywords
- composite fiber
- spinning
- cellulose base
- heat
- pva
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the field of manufacturing composite fiber membranes, and relates to a method for manufacturing a composite fiber membrane, in particular to a method for manufacturing a cellulose base heat-resisting nano-composite fiber membrane in an electrostatic spinning mode. The method aims at solving the technical problems that a PVA membrane obtained through an existing method is large in brittleness, hard to form and low in porosity. The method comprises the steps of 1, preparing a CNCs solution; 2, preparing an electrospinning solution; 3, putting the electrospinning solution into an injection syringe, and conducting spinning to obtain the cellulose base heat-resisting nano-composite fiber membrane. According to the method, the environment-friendly and efficient electrospinning technology is adopted for solving the problems that the PVA membrane is hard to form and the performance is not easy to control; the ultra-fine PVA/CNC nano-composite fiber with the smooth surface and the uniform diameter is obtained, and the using performance of the PVA membrane obtained through electrospinning is better.
Description
Technical field
The present invention relates to a kind of preparation method of composite fiber thin film.
Background technology
Polyvinyl alcohol (PVA) is a kind of water-soluble, hypocrystalline, nontoxic, degradable and biocompatible polymer, and therefore, it is with a wide range of applications.In addition, polyvinyl alcohol based nano-fiber has been widely used in the aspects such as tissue engineering bracket, filtering material, membrane material, protective clothing and medicament slow release.But the PVA film fragility that traditional film build method obtains is comparatively large, porosity is low and thermal property is poor, and thus its use is also subject to strict restriction.Therefore, the PVA film build method of research high-efficiency environment friendly, realizes the high performance of PVA material, has great importance.In numerous film build methods, the advantages such as method of electrostatic spinning is easy to operate by it, environmental protection become one of effective way of preparation High performance nanometer composite material, and the nanofiber prepared has that diameter is little, the interconnective network structure of high-ratio surface sum.Electrostatic spinning technique is introduced PVA film forming procedure, the PVA fiber membrane prepared has one-dimensional nano structure, diameter can reach hundreds of nanometer, achieve the preparation of ultra-fine PVA nano-composite fiber, particularly the medical character of PVA self is combined with the cancellated specific function of electrostatic spinning, also can prepare and there is highly porous thin-film material.
Nano-cellulose (CNCs) successfully prepares the novel nanocomposite materials of high-performance and wide application prospect with characteristics such as its outstanding mechanical performance, renewable and biodegradations, be added in PVA matrix, due to the hydrophily that the two is common, make it when blended, realize good interface cohesion, effectively can strengthen the properties of nano composite material.But, abundant not enough about the research of the thermal property of CNCs in PVA polymeric matrix, need further further investigation badly.
Summary of the invention
The object of the invention is to solve that PVA film fragility prepared by existing method is comparatively large, porosity is low and the technical problem of thermal property difference, provides the method for a kind of electro-spinning for the heat-resisting nano-composite fiber film of cellulose base.
Electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 130 ~ 220g sulphuric acid hydrolysis, 20 ~ 50g MCC1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 5 ~ 10 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then the CNCs of sedimentation is collected
By CNCs according to first centrifugal, add 5 ~ 10 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, be dissolved in 170 ~ 333g deionized water by 30 ~ 50gPVA particle, in 80 ~ 90 DEG C of water-baths, stir 2 ~ 3h to PVA particle all dissolve, leave standstill 12 ~ 24h, obtaining mass fraction is 10 ~ 20%PVA solution,
Take 30 ~ 70gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that CNC addition is 5 ~ 20%, after room temperature condition lower magnetic force stirs 12 ~ 24h, adopt ultrasonic cell disrupte machine process 5 ~ 10 minutes, obtain electrospinning liquid;
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 10 ~ 30kV, negative pressure is-1 ~-3kV, pushing away post speed is 0.6 ~ 1.5mm/min, and drum rotation speed is 20 ~ 120rpm, and the Electrospun time is 2 ~ 8 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Main purpose of the present invention overcomes technical barrier such as PVA conventional method film forming more crisp grade, discloses the preparation method of a kind of environmental protection, efficiently Novel static electrospinning PVA/CNCs nano-composite fiber film.The method adopts deionized water as solvent, will PVA dissolve after add the CNCs of different quality, mix and rear electrostatic spinning carried out to it.Contrast prior art, the electrospinning PVA/CNCs film adopting this method to prepare has the following advantages:
1, PVA film forming is difficult, the uppity problem of performance to adopt the Static Spinning technology of environment-friendly high-efficiency to solve;
2, prepare the ultra-fine PVA/CNC nano-composite fiber of smooth surface, uniform diameter, its higher porosity preferably has numerical value to impart the more excellent serviceability of electrospinning PVA film;
3, with the increase gradually of CNCs addition, improve the thermal property of PVA/CNCs film.The present invention will expand the practical application of Static Spinning PVA/CNCs nano-composite fiber thin film technique, and provide theoretical foundation for its correlative study.
Adopt method disclosed by the invention, environmental protection, the simple preparation realizing Static Spinning PVA/CNCs nano-composite fiber film efficiently, the thermal property of gained film improves.The high thermal property nano-composite fiber method for manufacturing thin film that the present invention announces, the configuration of electrospinning liquid is fast, preparation technology is simple, for correlative study provides theoretical foundation, have also increased dramatically range of application and the prospect of the application of PVA, the electrostatic spinning product obtained can be applicable to prepare the fields such as heat proof material simultaneously.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance figure of experiment one step one gained CNCs;
Fig. 2 is the electrospinning liquid photo of different CNCs addition and size in experiment one to experiment five;
Fig. 3 is that the electro-spinning of experiment one preparation is for cellulose base heat-resisting nano-composite fiber film microscopic appearance structure chart;
Fig. 4 is that the electro-spinning of experiment two preparation is for cellulose base heat-resisting nano-composite fiber film microscopic appearance structure chart;
Fig. 5 is that the electro-spinning of experiment three preparation is for cellulose base heat-resisting nano-composite fiber film microscopic appearance structure chart;
Fig. 6 is that the electro-spinning of experiment four preparation is for cellulose base heat-resisting nano-composite fiber film microscopic appearance structure chart;
Fig. 7 is that the electro-spinning of experiment five preparation is for cellulose base heat-resisting nano-composite fiber film microscopic appearance structure chart;
Fig. 8 is the FTIR collection of illustrative plates of electro-spinning for the heat-resisting nano-composite fiber film of cellulose base of preparation in experiment one to experiment five, the FTIR collection of illustrative plates of CNCs prepared by 1 expression experiment one step one in figure, the FTIR collection of illustrative plates of Static Spinning PVA fiber membrane prepared by 2 expression experiments one, 3 represent that electro-spinning prepared by experiments two is for the FTIR collection of illustrative plates of the heat-resisting nano-composite fiber film of cellulose base, 4 represent that electro-spinning prepared by experiments three is for the FTIR collection of illustrative plates of the heat-resisting nano-composite fiber film of cellulose base, 5 represent that electro-spinning prepared by experiments four is for the FTIR collection of illustrative plates of the heat-resisting nano-composite fiber film of cellulose base, 6 represent that electro-spinning prepared by experiments five is for the FTIR collection of illustrative plates of the heat-resisting nano-composite fiber film of cellulose base,
Fig. 9 is the TGA curve of electro-spinning for the heat-resisting nano-composite fiber film of cellulose base of preparation in experiment one to experiment five, the TGA curve of CNCs prepared by 1 expression experiment one step one in figure, the TGA curve of Static Spinning PVA fiber membrane prepared by 2 expression experiment one step 2, 3 represent that electro-spinning prepared by experiments two is for the TGA curve of the heat-resisting nano-composite fiber film of cellulose base, 4 represent that electro-spinning prepared by experiments three is for the TGA curve of the heat-resisting nano-composite fiber film of cellulose base, 5 represent that electro-spinning prepared by experiments four is for the TGA curve of the heat-resisting nano-composite fiber film of cellulose base, 6 represent that electro-spinning prepared by experiments five is for the TGA curve of the heat-resisting nano-composite fiber film of cellulose base,
Figure 10 is the DTG curve of electro-spinning for the heat-resisting nano-composite fiber film of cellulose base of preparation in experiment one to experiment five, the DTG curve of CNCs prepared by 1 expression experiment one step one in figure, the DTG curve of Static Spinning PVA fiber membrane prepared by 2 expression experiment one step 2, 3 represent that electro-spinning prepared by experiments two is for the DTG curve of the heat-resisting nano-composite fiber film of cellulose base, 4 represent that electro-spinning prepared by experiments three is for the DTG curve of the heat-resisting nano-composite fiber film of cellulose base, 5 represent that electro-spinning prepared by experiments four is for the DTG curve of the heat-resisting nano-composite fiber film of cellulose base, the DTG curve of the heat-resisting nano-composite fiber film of electrostatic spinning fiber element base prepared by 6 expression experiments five.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises any combination between each detailed description of the invention.
Detailed description of the invention one: in present embodiment, electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 130 ~ 220g sulphuric acid hydrolysis, 20 ~ 50g MCC (microcrystalline cellulose) 1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 5 ~ 10 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation
By CNCs according to first centrifugal, add 5 ~ 10 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, be dissolved in 170 ~ 333g deionized water by 30 ~ 50gPVA particle, in 80 ~ 90 DEG C of water-baths, stir 2 ~ 3h to PVA particle all dissolve, leave standstill 12 ~ 24h, obtaining mass fraction is 10 ~ 20%PVA solution,
Take 30 ~ 70gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that CNC addition is 5 ~ 20%, after room temperature condition lower magnetic force stirs 12 ~ 24h, adopt ultrasonic cell disrupte machine process 5 ~ 10 minutes, obtain electrospinning liquid;
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 10 ~ 30kV, negative pressure is-1 ~-3kV, pushing away post speed is 0.6 ~ 1.5mm/min, and drum rotation speed is 20 ~ 120rpm, and the Electrospun time is 2 ~ 8 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Detailed description of the invention two: present embodiment and detailed description of the invention one are 64% unlike the mass concentration of the sulfuric acid described in step one.Other is identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one or two, unlike the deionized water dilution mixture solution adding mixed solution quality 8 times in step one, obtain suspension.Other is identical with one of detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three stir in 85 DEG C of water-baths unlike in step 2.Other is identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are 10% unlike the mass fraction of CNC addition in step 2 PVA/CNCs mixed solution.Other is identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five are 15% unlike the mass fraction of CNC addition in step 2 PVA/CNCs mixed solution.Other is identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are 20kV unlike positive high voltage in step 3.Other is identical with one of detailed description of the invention one to six.
Detailed description of the invention eight: one of present embodiment and detailed description of the invention one to seven are-2kV unlike negative pressure in step 3.Other is identical with one of detailed description of the invention one to seven.
Detailed description of the invention nine: one of present embodiment and detailed description of the invention one to eight are 0.7mm/min unlike pushing away post speed in step 3.Other is identical with one of detailed description of the invention one to eight.
Detailed description of the invention ten: one of present embodiment and detailed description of the invention one to nine are 100rpm unlike step 3 intermediate roll rotating speed.Other is identical with one of detailed description of the invention one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
Electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 130g sulphuric acid hydrolysis 20g MCC1h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 5 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation,
By CNCs according to first centrifugal, add 5 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, 30gPVA particle is dissolved in 170g deionized water, in 80 DEG C of water-baths, stirs 2h to PVA particle all dissolve, leave standstill 12h, obtain PVA solution,
Three, adopt cylinder gathering-device, paste one deck aluminium foil (be about 240mm, wide be about 150mm) on its surface, CNCs solution is loaded in 2 ~ 25mL syringe, arranging positive high voltage is 10kV, and negative pressure is-1kV, and pushing away post speed is 0.6mm/min, drum rotation speed is 20rpm, the Electrospun time is 2 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, after spinning, obtain the heat-resisting nano-composite fiber film of cellulose base.
Experiment two:
Electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 140g sulphuric acid hydrolysis 30g MCC1.5h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 6 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation,
By CNCs according to first centrifugal, add 6 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, 40gPVA particle is dissolved in 180g deionized water, in 85 DEG C of water-baths, stirs 2.5h to PVA particle all dissolve, leave standstill 15h, obtain PVA solution,
Take the PVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that PVA mass fraction is 5%, after room temperature condition lower magnetic force stirs 16h, adopt ultrasonic cell disrupte machine process 5 minutes, obtain electrospinning liquid (PVA/CNC
64-5);
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 15kV, negative pressure is-2kV, pushing away post speed is 0.8mm/min, and drum rotation speed is 50rpm, and the Electrospun time is 4 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Experiment three:
Electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 180g sulphuric acid hydrolysis 25g MCC1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 8 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation,
By CNCs according to first centrifugal, add 8 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, 35gPVA particle is dissolved in 200g deionized water, in 84 DEG C of water-baths, stirs 3h to PVA particle all dissolve, leave standstill 16h, obtain PVA solution,
Take the 50gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that PVA mass fraction is 10%, after room temperature condition lower magnetic force stirs 18h, adopt ultrasonic cell disrupte machine process 7 minutes, obtain electrospinning liquid (PVA/CNC
64-10);
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 20kV, negative pressure is-3kV, pushing away post speed is 1mm/min, and drum rotation speed is 80rpm, and the Electrospun time is 5 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Experiment four:
Electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 210g sulphuric acid hydrolysis 45g MCC1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 10 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation,
By CNCs according to first centrifugal, add 7 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, 40gPVA particle is dissolved in 230g deionized water, in 86 DEG C of water-baths, stirs 3h to PVA particle all dissolve, leave standstill 20h, obtain PVA solution,
Take the 70gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that PVA mass fraction is 15%, after room temperature condition lower magnetic force stirs 24h, adopt ultrasonic cell disrupte machine process 8 minutes, obtain electrospinning liquid (PVA/CNC
64-15);
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 30kV, negative pressure is-3kV, pushing away post speed is 1.5mm/min, and drum rotation speed is 120rpm, and the Electrospun time is 8 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Experiment five:
One, under 45 DEG C of water bath condition, adopt 210g sulphuric acid hydrolysis 45g MCC1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 10 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then collect the CNCs of sedimentation,
By CNCs according to first centrifugal, add 10 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, 40gPVA particle is dissolved in 230g deionized water, in 86 DEG C of water-baths, stirs 3h to PVA particle all dissolve, leave standstill 20h, obtain PVA solution,
Take the 70gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that PVA mass fraction is 20%, after room temperature condition lower magnetic force stirs 24h, adopt ultrasonic cell disrupte machine process 9 minutes, obtain electrospinning liquid (PVA/CNC
64-20);
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 30kV, negative pressure is-3kV, pushing away post speed is 1.5mm/min, and drum rotation speed is 120rpm, and the Electrospun time is 8 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
Find out the transparency of solution increasing and weaken gradually with CNCs by Fig. 2, increase with CNCs size and become white from light blue.
From Fig. 3 to Fig. 5, the increase of known CNCs addition does not have fiber morphology affects more significantly, and the smooth and diameter of the fiber formed is evenly distributed, and diameter is about 200 ~ 500nm.
Test the viscosity of the spinning solution for preparing to experiment, surface tension and electrical conductivity as table 1:
Measure at 25 DEG C.
Claims (10)
1. electro-spinning is for the method for the heat-resisting nano-composite fiber film of cellulose base, it is characterized in that electro-spinning is as follows for the method for cellulose base heat-resisting nano-composite fiber film:
One, under 45 DEG C of water bath condition, adopt 130 ~ 220g sulphuric acid hydrolysis, 20 ~ 50g MCC1 ~ 2h, obtain mixed solution, add the deionized water dilution mixture solution of mixed solution quality 5 ~ 10 times, obtain suspension, by suspension at 4 DEG C of standing 24h, then the CNCs of sedimentation is collected
By CNCs according to first centrifugal, add 5 ~ 10 times of deionized waters dilutions operation in tandem centrifugal again 3 times again, collect 3 times centrifugal after the faintly acid CNC aqueous solution, be placed in bag filter and dialyse to pH value to be 7, to obtain CNCs solution;
Two, be dissolved in 170 ~ 333g deionized water by 30 ~ 50gPVA particle, in 80 ~ 90 DEG C of water-baths, stir 2 ~ 3h to PVA particle all dissolve, leave standstill 12 ~ 24h, obtaining mass fraction is 10 ~ 20%PVA solution,
Take 30 ~ 70gPVA aqueous solution to mix with CNCs solution, obtain the PVA/CNCs mixed solution that CNC addition is 5 ~ 20%, after room temperature condition lower magnetic force stirs 12 ~ 24h, adopt ultrasonic cell disrupte machine process 5 ~ 10 minutes, obtain electrospinning liquid;
Three, electrospinning liquid is loaded in syringe, arranging positive high voltage is 10 ~ 30kV, negative pressure is-1 ~-3kV, pushing away post speed is 0.6 ~ 1.5mm/min, and drum rotation speed is 20 ~ 120rpm, and the Electrospun time is 2 ~ 8 hours, electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning, obtains the heat-resisting nano-composite fiber film of cellulose base.
2. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that the mass concentration of the sulfuric acid described in step one is 64% according to claim 1.
3. according to claim 1 or 2, electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that the deionized water dilution mixture solution adding mixed solution quality 8 times in step one, obtains suspension.
4. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that stirring in 85 DEG C of water-baths in step 2 according to claim 1.
5. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that the mass fraction of CNC addition in step 2 PVA/CNCs mixed solution is 10% according to claim 1.
6. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that the mass fraction of CNC addition in step 2 PVA/CNCs mixed solution is 15% according to claim 1.
7. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that in step 3, positive high voltage is 20kV according to claim 1.
8. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that in step 3, negative pressure is-2kV according to claim 1.
9. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that pushing away post speed in step 3 is 0.7mm/min according to claim 1.
10. electro-spinning, for the method for the heat-resisting nano-composite fiber film of cellulose base, is characterized in that step 3 intermediate roll rotating speed is 100rpm according to claim 1.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510415614.0A CN104928849B (en) | 2015-07-15 | 2015-07-15 | Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201510415614.0A CN104928849B (en) | 2015-07-15 | 2015-07-15 | Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base |
Publications (2)
Publication Number | Publication Date |
---|---|
CN104928849A true CN104928849A (en) | 2015-09-23 |
CN104928849B CN104928849B (en) | 2017-03-29 |
Family
ID=54116263
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201510415614.0A Expired - Fee Related CN104928849B (en) | 2015-07-15 | 2015-07-15 | Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104928849B (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106511318A (en) * | 2016-10-10 | 2017-03-22 | 北京科技大学 | Preparing method for nano-composite fiber film with functions of carrying medicine and killing cancer cells |
CN108250460A (en) * | 2018-02-01 | 2018-07-06 | 浙江纺织服装职业技术学院 | A kind of preparation method and application of cellulose solution |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102423506A (en) * | 2011-12-09 | 2012-04-25 | 东华大学 | Medicine sustained release nanofiber membrane for treating periodontitis and preparation method for medicine sustained release nanofiber membrane |
CN103866487A (en) * | 2014-03-27 | 2014-06-18 | 同济大学 | Method for preparing NCC/CS/PVA composite nano-membrane |
CN103882624A (en) * | 2014-03-27 | 2014-06-25 | 同济大学 | Preparation method for water-resistant nano microcrystalline cellulose/polyvinyl alcohol/polyacrylic acid/silicon dioxide composite nanofiber membrane |
CN104562442A (en) * | 2015-02-05 | 2015-04-29 | 东北林业大学 | Method for preparing cellulose based nano-composite fiber membrane through electrostatic spinning |
-
2015
- 2015-07-15 CN CN201510415614.0A patent/CN104928849B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102423506A (en) * | 2011-12-09 | 2012-04-25 | 东华大学 | Medicine sustained release nanofiber membrane for treating periodontitis and preparation method for medicine sustained release nanofiber membrane |
CN103866487A (en) * | 2014-03-27 | 2014-06-18 | 同济大学 | Method for preparing NCC/CS/PVA composite nano-membrane |
CN103882624A (en) * | 2014-03-27 | 2014-06-25 | 同济大学 | Preparation method for water-resistant nano microcrystalline cellulose/polyvinyl alcohol/polyacrylic acid/silicon dioxide composite nanofiber membrane |
CN104562442A (en) * | 2015-02-05 | 2015-04-29 | 东北林业大学 | Method for preparing cellulose based nano-composite fiber membrane through electrostatic spinning |
Non-Patent Citations (2)
Title |
---|
QINGFENG SHIA, CHENGJUN ZHOU, YIYING YUE, WEIHONG GUO: "Mechanical properties and in vitro degradation of electrospun", 《CARBOHYDRATE POLYMERS》 * |
戴磊,龙柱: "纳米纤维素增强聚乙烯醇/水性聚氨酯静电纺膜的研究", 《功能科技》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106511318A (en) * | 2016-10-10 | 2017-03-22 | 北京科技大学 | Preparing method for nano-composite fiber film with functions of carrying medicine and killing cancer cells |
CN106511318B (en) * | 2016-10-10 | 2019-04-02 | 北京科技大学 | Preparation method with the nano-composite fiber film for carrying medicine and killing cancer cell |
CN108250460A (en) * | 2018-02-01 | 2018-07-06 | 浙江纺织服装职业技术学院 | A kind of preparation method and application of cellulose solution |
CN108250460B (en) * | 2018-02-01 | 2021-07-30 | 浙江纺织服装职业技术学院 | Preparation method and application of cellulose solution |
Also Published As
Publication number | Publication date |
---|---|
CN104928849B (en) | 2017-03-29 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103866487B (en) | The preparation method of a kind of nano micro crystal cellulose/chitosan/polyvinyl alcohol composite nanometer film | |
CN102013516B (en) | Porous fiber gel polymer electrolyte and preparation method thereof | |
CN103147355B (en) | A kind of preparation method of biomass nano fiber conductive paper | |
CN103993380B (en) | A kind of preparation method of Chitosan Fiber With High Tenacity | |
CN105239184A (en) | Bacterial cellulose/graphene/ferroferric oxide composite film and preparation method thereof | |
CN104878590A (en) | Preparation method of conductive graphene nanofiber membrane | |
CN103319731B (en) | Regenerated silk fibroin solution and preparation method thereof | |
CN103882624B (en) | The preparation method of WATER RESISTANCE nano micro crystal cellulose/polyvinyl alcohol/polyacrylic acid/silica composite nano-fiber membrane | |
CN104790067A (en) | Nano conductive polymer/graphene composite fiber, and preparation method and application thereof | |
CN109537163B (en) | Chitosan/sodium alginate/polyvinyl alcohol polyelectrolyte nanofiber composite membrane and preparation method thereof | |
CN104916448A (en) | Hierarchical structure micro-nano porous fiber electrode material and preparing method thereof | |
CN103346281A (en) | Sodium alginate-based lithium battery diaphragm and preparation method thereof | |
CN104562292A (en) | Preparation method of porous micro-nano PET fibers | |
CN104963098A (en) | Method for preparing electrostatic spinning perfluocarbon polymer nanofiber membrane | |
WO2017214741A1 (en) | Process for preparing chitosan/polyvinyl alcohol composite electrically-conductive nanofibre | |
CN103483606A (en) | Preparation method of bacterial cellulose composite polymer superfine fiber material | |
CN102587039A (en) | High-temperature-resistance zinc titanate/silicon dioxide protection material and preparation method therefor | |
CN102586928B (en) | Polyvinyl alcohol nanofiber, and preparation method and device thereof | |
CN103865104B (en) | A kind of preparation method of core shell nanoparticles | |
CN111020745A (en) | Preparation method of sodium alginate and chitosan composite nanofiber | |
CN104928849A (en) | Method for manufacturing cellulose base heat-resisting nano-composite fiber membrane in electrostatic spinning mode | |
CN104562442B (en) | Electrostatic spinning prepares the method for cellulose based nano composite fiber thin film | |
CN105506858A (en) | Method for preparing cellulose-reinforced nano-composite fiber membrane by electrostatic spinning | |
CN104733190A (en) | Composite diaphragm and manufacturing method thereof | |
CN113186656A (en) | Carbon nitride-polyvinyl alcohol composite antibacterial film and preparation method and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170329 Termination date: 20190715 |