CN104928849B - Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base - Google Patents

Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base Download PDF

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CN104928849B
CN104928849B CN201510415614.0A CN201510415614A CN104928849B CN 104928849 B CN104928849 B CN 104928849B CN 201510415614 A CN201510415614 A CN 201510415614A CN 104928849 B CN104928849 B CN 104928849B
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thin film
composite fiber
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CN104928849A (en
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宦思琪
韩广萍
程万里
白龙
李超
刘国相
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Northeast Forestry University
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Abstract

Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base, it is related to a kind of preparation method of composite fiber thin film.The present invention's is in order to the larger film forming of PVA film fragility for solving existing method preparation is difficult, the technical problem that porosity is low.This method:First, prepare CNCs solution;2nd, prepare electrospinning liquid;3rd, by electrospinning liquid loaded in syringe, spinning obtains the heat-resisting nano-composite fiber thin film of cellulose base.The present invention solves PVA film forming hardly possible, the uppity problem of performance using the electrostatic spinning technique of environment-friendly high-efficiency;Prepare that surface is smooth, uniform diameter ultra-fine PVA/CNC nano-composite fibers, impart the more excellent performance of electrospinning PVA film.The invention belongs to the preparation field of composite fiber thin film.

Description

Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base
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, therefore, Which is with a wide range of applications.Additionally, polyvinyl alcohol based nano-fiber has been widely used for tissue engineering bracket, filter material The aspects such as material, membrane material, protective garment and medicament slow release.However, PVA film fragility that traditional film build method is obtained is larger, hole Gap rate is low and thermal property is poor, thus its use is also severely limited.Therefore, the PVA film build methods of high-efficiency environment friendly are studied, it is real The high performance of existing PVA materials, has great importance.In numerous film build methods, method of electrostatic spinning is by its easy to operate, ring The advantages of guarantor, becomes one of effective way of preparation High performance nanometer composite material, and the nanofiber for preparing has diameter Little, high-specific surface area and the network structure being connected with each other.Electrostatic spinning technique is introduced into PVA film forming procedures, the PVA for preparing is fine Dimension thin film has one-dimensional nano structure, and diameter realizes the preparation of ultra-fine PVA nano-composite fibers, especially up to hundreds of nanometer It is that the medical property of PVA itself is combined with the cancellated specific function of electrostatic spinning, can also prepares with high hole The thin-film material of degree.
Nano-cellulose (CNCs) is successfully prepared with characteristics such as its outstanding mechanical performance, renewable and biodegradations The novel nanocomposite materials of high-performance and wide application prospect, are added in PVA matrixes, as the two is common hydrophilic Property so as to good interface cohesion is realized in blending, can effectively strengthen the properties of nano composite material.But, close It is abundant not enough in the research of thermal properties of the CNCs in PVA polymeric matrixs, need badly and further further investigate.
The content of the invention
The invention aims to solve existing method preparation PVA film fragility is larger, porosity is low and calorifics A kind of technical problem of energy difference, there is provided method of electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base.
Electro-spinning is as follows for the method for the heat-resisting nano-composite fiber thin film of cellulose base:
First, under 45 DEG C of water bath conditions, using 130~220g sulphuric acid hydrolysis, 20~50g MCC1~2h, obtain mixing molten Liquid, adds the deionized water dilution mixture solution of 5~10 times of mixed solution quality, obtains suspension, and suspension is stood at 4 DEG C 24h, then collects the CNCs of sedimentation,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 5~10 times of deionized waters is centrifuged again, is collected 3 times Faintly acid CNC aqueous solution after centrifugation, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 30~50gPVA granules are dissolved in 170~333g deionized waters, in 80~90 DEG C of water-baths stirring 2~ 3h to PVA granules all dissolve, and stand 12~24h, and it is 10~20%PVA solution to obtain mass fraction,
Weigh 30~70gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs that CNC additions are 5~20% and mix Solution is closed, after 12~24h of magnetic agitation under room temperature condition, is processed 5~10 minutes using ultrasonic cell disrupte machine, is obtained electrospinning Liquid;
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 10~30kV, and negative pressure is -1~-3kV, pushes away post speed For 0.6~1.5mm/min, drum rotation speed is 20~120rpm, and the Electrospun time is 2~8 hours, and electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning is finished, obtains the heat-resisting nano-composite fiber thin film of cellulose base.
The main object of the present invention is to overcome the more crisp grade technical barrier of PVA traditional method film forming, discloses a kind of environmental protection, height The preparation method of the novel static electrospinning PVA/CNCs nano-composite fiber thin film of effect.The method adopts deionized water as solvent, The CNCs of different quality is added after PVA is dissolved, electrostatic spinning is carried out to which after mix homogeneously.Contrast prior art, using this Electrospinning PVA/CNCs thin film prepared by method has advantages below:
1st, PVA film forming hardly possible, the uppity problem of performance are solved using the electrostatic spinning technique of environment-friendly high-efficiency;
2nd, prepare that surface is smooth, uniform diameter ultra-fine PVA/CNC nano-composite fibers, its higher porosity is best There is numerical value to impart the more excellent performance of electrospinning PVA film;
3rd, with the gradually increase of CNCs additions, improve the thermal property of PVA/CNCs thin film.The present invention will expand quiet The practical application of electrospinning PVA/CNCs nano-composite fiber thin film technique, and theoretical foundation is provided for its correlational study.
Using method disclosed by the invention, environmental protection, the nano combined fibres of Static Spinning PVA/CNCs are simply and efficiently realized The preparation of dimension thin film, the thermal property of gained thin film are improved.The high thermal property nano-composite fiber thin film announced by the present invention Preparation method, the configuration of electrospinning liquid are fast, and preparation process is simple provides theoretical foundation for correlational study, while also greatly increasing The range of application and prospect of the application of PVA, resulting electrostatic spinning product can be applicable to prepare the fields such as heat proof material.
Description of the drawings
Fig. 1 is the microscopic appearance figure for testing a step one gained CNCs;
Fig. 2 is to test one to the electrospinning liquid photo for testing difference CNCs additions and size in five;
Fig. 3 is to test an electro-spinning for preparing for the heat-resisting nano-composite fiber thin film microscopic appearance structure of cellulose base Figure;
Fig. 4 is to test two electro-spinnings for preparing for the heat-resisting nano-composite fiber thin film microscopic appearance structure of cellulose base Figure;
Fig. 5 is to test three electro-spinnings for preparing for the heat-resisting nano-composite fiber thin film microscopic appearance structure of cellulose base Figure;
Fig. 6 is to test four electro-spinnings for preparing for the heat-resisting nano-composite fiber thin film microscopic appearance structure of cellulose base Figure;
Fig. 7 is to test five electro-spinnings for preparing for the heat-resisting nano-composite fiber thin film microscopic appearance structure of cellulose base Figure;
Fig. 8 is to test an electro-spinning prepared into experiment five for the heat-resisting nano-composite fiber thin film of cellulose base FTIR collection of illustrative plates, in figure, 1 represents the FTIR collection of illustrative plates of CNCs prepared by one step one of experiment, and 2 represent Static Spinning PVA prepared by experiment one The FTIR collection of illustrative plates of fiber membrane, 3 represent the electro-spinning of two preparation of experiment for the heat-resisting nano-composite fiber thin film of cellulose base FTIR collection of illustrative plates, the FTIR collection of illustrative plates of electro-spinnings prepared by 4 expression experiments three for the heat-resisting nano-composite fiber thin film of cellulose base, 5 The FTIR collection of illustrative plates of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base of four preparation of experiment is represented, 6 represent experiment five FTIR collection of illustrative plates of the electro-spinning of preparation for the heat-resisting nano-composite fiber thin film of cellulose base;
Fig. 9 is to test an electro-spinning prepared into experiment five for the heat-resisting nano-composite fiber thin film of cellulose base TGA curves, in figure, 1 represents the TGA curves of CNCs prepared by one step one of experiment, and 2 represent electrostatic prepared by one step 2 of experiment The TGA curves of PVA fiber membranes are spun, 3 represent that electro-spinning prepared by experiment two is thin for the heat-resisting nano-composite fiber of cellulose base The TGA curves of film, 4 represent the TGA curve of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base of three preparation of experiment, 5 TGA curves of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base for representing four preparation of experiment, 6 represent experiment five TGA curve of the electro-spinning of preparation for the heat-resisting nano-composite fiber thin film of cellulose base;
Figure 10 is to test an electro-spinning prepared into experiment five for the heat-resisting nano-composite fiber thin film of cellulose base DTG curves, in figure, 1 represents the DTG curves of CNCs prepared by one step one of experiment, and 2 represent electrostatic prepared by one step 2 of experiment The DTG curves of PVA fiber membranes are spun, 3 represent that electro-spinning prepared by experiment two is thin for the heat-resisting nano-composite fiber of cellulose base The DTG curves of film, 4 represent the DTG curve of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base of three preparation of experiment, 5 DTG curves of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base for representing four preparation of experiment, 6 represent experiment five The DTG curves of the heat-resisting nano-composite fiber thin film of electrostatic spinning fiber element base of preparation.
Specific embodiment
Technical solution of the present invention is not limited to act specific embodiment set forth below, also including between each specific embodiment Combination in any.
Specific embodiment one:Side of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base in present embodiment Method is as follows:
First, under 45 DEG C of water bath conditions, using 130~220g sulphuric acid hydrolysis 20~50g MCC (Microcrystalline Cellulose) 1~ 2h, obtains mixed solution, adds the deionized water dilution mixture solution of 5~10 times of mixed solution quality, obtains suspension, will suspend Liquid stands 24h at 4 DEG C, then collects the CNCs of sedimentation,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 5~10 times of deionized waters is centrifuged again, is collected 3 times Faintly acid CNC aqueous solution after centrifugation, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 30~50gPVA granules are dissolved in 170~333g deionized waters, in 80~90 DEG C of water-baths stirring 2~ 3h to PVA granules all dissolve, and stand 12~24h, and it is 10~20%PVA solution to obtain mass fraction,
Weigh 30~70gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs that CNC additions are 5~20% and mix Solution is closed, after 12~24h of magnetic agitation under room temperature condition, is processed 5~10 minutes using ultrasonic cell disrupte machine, is obtained electrospinning Liquid;
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 10~30kV, and negative pressure is -1~-3kV, pushes away post speed For 0.6~1.5mm/min, drum rotation speed is 20~120rpm, and the Electrospun time is 2~8 hours, and electrospinning the temperature inside the box is 25 DEG C, humidity is 13%, after spinning is finished, obtains the heat-resisting nano-composite fiber thin film of cellulose base.
Specific embodiment two:Present embodiment and the sulphuric acid unlike specific embodiment one described in step one Mass concentration is 64%.Other are identical with specific embodiment one.
Specific embodiment three:Add in step one unlike one of present embodiment and specific embodiment one or two The deionized water dilution mixture solution of 8 times of mixed solution quality, obtains suspension.Other phases one of with specific embodiment one or two Together.
Specific embodiment four:In 85 in step 2 unlike one of present embodiment and specific embodiment one to three Stir in DEG C water-bath.Other are identical with one of specific embodiment one to three.
Specific embodiment five:Step 2 PVA/ unlike one of present embodiment and specific embodiment one to four In CNCs mixed solutions, the mass fraction of CNC additions is 10%.Other are identical with one of specific embodiment one to four.
Specific embodiment six:Step 2 PVA/ unlike one of present embodiment and specific embodiment one to five In CNCs mixed solutions, the mass fraction of CNC additions is 15%.Other are identical with one of specific embodiment one to five.
Specific embodiment seven:It is positive high in step 3 unlike one of present embodiment and specific embodiment one to six Press as 20kV.Other are identical with one of specific embodiment one to six.
Specific embodiment eight:Negative pressure in step 3 unlike one of present embodiment and specific embodiment one to seven For -2kV.Other are identical with one of specific embodiment one to seven.
Specific embodiment nine:Post is pushed away in step 3 unlike one of present embodiment and specific embodiment one to eight Speed is 0.7mm/min.Other are identical with one of specific embodiment one to eight.
Specific embodiment ten:Step 3 intermediate roll unlike one of present embodiment and specific embodiment one to nine Rotating speed is 100rpm.Other are identical with one of specific embodiment one to nine.
Using following experimental verifications effect of the present invention:
Experiment one:
Electro-spinning is as follows for the method for the heat-resisting nano-composite fiber thin film of cellulose base:
First, under 45 DEG C of water bath conditions, using 130g sulphuric acid hydrolysis 20g MCC1h, mixed solution is obtained, adds mixing molten The deionized water dilution mixture solution of 5 times of liquid quality, obtains suspension, and suspension is stood 24h at 4 DEG C, then collects sedimentation CNCs,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 5 times of deionized waters is centrifuged again, 3 centrifugations are collected Faintly acid CNC aqueous solution afterwards, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 30gPVA granules are dissolved in 170g deionized waters, 2h to PVA granules are stirred in 80 DEG C of water-baths all molten Solution, stands 12h, obtains PVA solution,
3rd, using cylinder collection device, one layer of aluminium foil (being about 240mm, wide about 150mm) is pasted on its surface, by CNCs Loaded in 2~25mL syringes, setting positive high voltage is 10kV to solution, and negative pressure is -1kV, pushes away post speed for 0.6mm/min, cylinder Rotating speed is 20rpm, and the Electrospun time is 2 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, after spinning is finished, obtains fibre The heat-resisting nano-composite fiber thin film of the plain base of dimension.
Experiment two:
Electro-spinning is as follows for the method for the heat-resisting nano-composite fiber thin film of cellulose base:
First, under 45 DEG C of water bath conditions, using 140g sulphuric acid hydrolysis 30g MCC1.5h, mixed solution is obtained, adds mixing The deionized water dilution mixture solution of 6 times of solution quality, obtains suspension, and suspension is stood 24h at 4 DEG C, then collects sedimentation CNCs,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 6 times of deionized waters is centrifuged again, 3 centrifugations are collected Faintly acid CNC aqueous solution afterwards, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 40gPVA granules are dissolved in 180g deionized waters, 2.5h to PVA granule wholes is stirred in 85 DEG C of water-baths Dissolving, stands 15h, obtains PVA solution,
Weigh PVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs mixed solutions that PVA mass fractions are 5%, in Under room temperature condition after magnetic agitation 16h, processed 5 minutes using ultrasonic cell disrupte machine, obtain electrospinning liquid (PVA/CNC64-5);
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 15kV, and negative pressure is -2kV, pushes away post speed for 0.8mm/ Min, drum rotation speed are 50rpm, and the Electrospun time is 4 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, and spinning is finished Afterwards, obtain the heat-resisting nano-composite fiber thin film of cellulose base.
Experiment three:
Electro-spinning is as follows for the method for the heat-resisting nano-composite fiber thin film of cellulose base:
First, under 45 DEG C of water bath conditions, using 180g sulphuric acid hydrolysis 25g MCC1~2h, mixed solution is obtained, is added mixed The deionized water dilution mixture solution of 8 times of solution quality is closed, suspension is obtained, suspension is stood into 24h at 4 DEG C, then collect heavy The CNCs of drop,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 8 times of deionized waters is centrifuged again, 3 centrifugations are collected Faintly acid CNC aqueous solution afterwards, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 35gPVA granules are dissolved in 200g deionized waters, 3h to PVA granules are stirred in 84 DEG C of water-baths all molten Solution, stands 16h, obtains PVA solution,
Weigh 50gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs mixing that PVA mass fractions are 10% molten Liquid, after magnetic agitation 18h under room temperature condition, is processed 7 minutes using ultrasonic cell disrupte machine, obtains electrospinning liquid (PVA/ CNC64-10);
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 20kV, and negative pressure is -3kV, pushes away post speed for 1mm/ Min, drum rotation speed are 80rpm, and the Electrospun time is 5 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, and spinning is finished Afterwards, obtain the heat-resisting nano-composite fiber thin film of cellulose base.
Experiment four:
Electro-spinning is as follows for the method for the heat-resisting nano-composite fiber thin film of cellulose base:
First, under 45 DEG C of water bath conditions, using 210g sulphuric acid hydrolysis 45g MCC1~2h, mixed solution is obtained, is added mixed The deionized water dilution mixture solution of 10 times of solution quality is closed, suspension is obtained, suspension is stood into 24h at 4 DEG C, then collect heavy The CNCs of drop,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 7 times of deionized waters is centrifuged again, 3 centrifugations are collected Faintly acid CNC aqueous solution afterwards, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 40gPVA granules are dissolved in 230g deionized waters, 3h to PVA granules are stirred in 86 DEG C of water-baths all molten Solution, stands 20h, obtains PVA solution,
Weigh 70gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs mixing that PVA mass fractions are 15% molten Liquid, after magnetic agitation 24h under room temperature condition, is processed 8 minutes using ultrasonic cell disrupte machine, obtains electrospinning liquid (PVA/ CNC64-15);
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 30kV, and negative pressure is -3kV, pushes away post speed for 1.5mm/ Min, drum rotation speed are 120rpm, and the Electrospun time is 8 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, and spinning is finished Afterwards, obtain the heat-resisting nano-composite fiber thin film of cellulose base.
Experiment five:
First, under 45 DEG C of water bath conditions, using 210g sulphuric acid hydrolysis 45g MCC1~2h, mixed solution is obtained, is added mixed The deionized water dilution mixture solution of 10 times of solution quality is closed, suspension is obtained, suspension is stood into 24h at 4 DEG C, then collect heavy The CNCs of drop,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 10 times of deionized waters is centrifuged again, collect 3 times from Faintly acid CNC aqueous solution after the heart, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 40gPVA granules are dissolved in 230g deionized waters, 3h to PVA granules are stirred in 86 DEG C of water-baths all molten Solution, stands 20h, obtains PVA solution,
Weigh 70gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs mixing that PVA mass fractions are 20% molten Liquid, after magnetic agitation 24h under room temperature condition, is processed 9 minutes using ultrasonic cell disrupte machine, obtains electrospinning liquid (PVA/ CNC64-20);
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 30kV, and negative pressure is -3kV, pushes away post speed for 1.5mm/ Min, drum rotation speed are 120rpm, and the Electrospun time is 8 hours, and electrospinning the temperature inside the box is 25 DEG C, and humidity is 13%, and spinning is finished Afterwards, obtain the heat-resisting nano-composite fiber thin film of cellulose base.
Find out that by Fig. 2 the transparency of solution gradually weakens with increasing for CNCs, increase by pale blue complexion changed with CNCs sizes For white.
Understand that from Fig. 3 to Fig. 5 the increase of CNCs additions does not have more significant impact, the fibre for being formed to fiber morphology Dimension is smooth and diameter Distribution is uniform, and diameter is 200~500nm or so.
Experiment one is to viscosity, surface tension and the electrical conductivity such as table 1 for testing the spinning liquid for preparing:
Measure at 25 DEG C.

Claims (10)

1. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base, it is characterised in that electro-spinning is for cellulose The method of the heat-resisting nano-composite fiber thin film of base is as follows:
First, under 45 DEG C of water bath conditions, using 130~220g sulphuric acid hydrolysis, 20~50g MCC1~2h, mixed solution is obtained, plus Enter the deionized water dilution mixture solution of 5~10 times of mixed solution quality, obtain suspension, suspension is stood into 24h at 4 DEG C, so The CNCs of sedimentation is collected afterwards,
CNCs is operated 3 times according to being first centrifuged, adding the order that the dilution of 5~10 times of deionized waters is centrifuged again, 3 centrifugations are collected Faintly acid CNC aqueous solution afterwards, be placed in bag filter dialyse to pH value be 7, obtain CNCs solution;
2nd, 30~50gPVA granules are dissolved in 170~333g deionized waters, 2~3h is stirred extremely in 80~90 DEG C of water-baths PVA granules all dissolve, and stand 12~24h, and it is 10~20%PVA solution to obtain mass fraction,
Weigh 30~70gPVA aqueous solutions to mix with CNCs solution, obtain the PVA/CNCs mixing that CNC additions are 5~20% molten Liquid, after 12~24h of magnetic agitation under room temperature condition, is processed 5~10 minutes using ultrasonic cell disrupte machine, obtains electrospinning liquid;
3rd, by electrospinning liquid loaded in syringe, setting positive high voltage is 10~30kV, and negative pressure is -1~-3kV, pushes away post speed for 0.6 ~1.5mm/min, drum rotation speed are 20~120rpm, and the Electrospun time is 2~8 hours, and electrospinning the temperature inside the box is 25 DEG C, humidity For 13%, after spinning is finished, the heat-resisting nano-composite fiber thin film of cellulose base is obtained.
2. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist The mass concentration of the sulphuric acid described in step one is 64%.
3. method of the electro-spinning according to claim 1 or claim 2 for the heat-resisting nano-composite fiber thin film of cellulose base, its feature It is the deionized water dilution mixture solution of 8 times of addition mixed solution quality in step one, obtains suspension.
4. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist Stir in 85 DEG C of water-baths in step 2.
5. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist In step 2 PVA/CNCs mixed solution, the mass fraction of CNC additions is 10%.
6. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist In step 2 PVA/CNCs mixed solution, the mass fraction of CNC additions is 15%.
7. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist In step 3, positive high voltage is 20kV.
8. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist In step 3, negative pressure is -2kV.
9. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist Post speed is pushed away in step 3 for 0.7mm/min.
10. method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base according to claim 1, its feature exist In step 3 intermediate roll rotating speed be 100rpm.
CN201510415614.0A 2015-07-15 2015-07-15 Method of the electro-spinning for the heat-resisting nano-composite fiber thin film of cellulose base Expired - Fee Related CN104928849B (en)

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