CN101497701A - Preparation of multi-wall carbon nano-tube / dodecyl sodium sulfonate / polyvinyl alcohol compound film - Google Patents
Preparation of multi-wall carbon nano-tube / dodecyl sodium sulfonate / polyvinyl alcohol compound film Download PDFInfo
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Abstract
The invention relates to the preparation method of a multi-walled carbon nano-tube/dodecyl sodium sulfate/polyvinyl alcohol coextruded film, which comprises the following steps: distilled water solution A of polyvinyl alcohol with 5-15wt percentage by weight is prepared; distilled water solution of dodecyl sodium sulfate with 1wt percentage by weight is prepared, the purified multi-walled carbon nano-tube is dispersed in the distilled water solution of dodecyl sodium sulfate by a sonic oscillation way to obtain MWCNTs suspending liquid B with the content of 0.1-1 wt percent; the solution A and the suspending liquid B are evenly mixed to obtain mother solution C of MWCNTs/SDS/PVA coextruded film material with the content of 0.1-2 wt percent; and the mother solution C is prepared to the film on clean and dry glass film plates by a scraping way. The MWCNTs crude product is prepared by adopting the method of catalytic pyrolysis methane, thereby having low cost; the main solution is distilled water, thereby having no pollution on environment; the MWCNTs/SDS/PVA coextruded film not only has obviously enhanced mechanical property and electrical property, improved thermal stability and ventilation property, but also has greatly enhanced stability in an ultra-low temperature environment (liquid nitrogen temperature).
Description
Technical field
The invention belongs to the nano composite film technical field, particularly relate to a kind of preparation method of multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film.
Background technology
Multi-walled carbon nano-tubes (MWCNTs) has excellent mechanics, optical property and favorable conductive, heat conductivility; Its excellent mechanical property can be improved the intensity and the toughness of polymer composites well, meanwhile its excellent optical property can prepare novel optic polymer matrix material, its excellent conducting performance can be improved the specific conductivity of polymer materials again, and its good heat-conducting then can be improved the thermostability of polymer materials.The research of MWCNTs/ polymer composites has become an importance of nano composite material research field.
The preparation method of MWCNTs/ polymer composites mainly contains electrochemical in-situ polymerization, solution mixing method, situ aggregation method, melting mixing method etc., and mainly characteristics and the performance according to polymeric matrix decides.
Polyvinyl alcohol (PVA) is a kind of water-soluble polymers that contains a large amount of strongly hydrophilic groups, has good film-forming properties.Characteristics such as that its film has is transparent, resistance oxygen, oil resistance, antistatic, intensity height are widely used in the fields such as base material of the polaroid that wrapping material, biodegradable material and liquid-crystal display use.But shortcomings such as that PVA exists is water-fast, resistance toheat difference have seriously hindered it and have used widely.MWCNTs and PVA be compounded with may obtain performance significantly or the composite film material that obviously improves, range of application will be more extensive.
Sodium laurylsulfonate (SDS) is a kind of anion surfactant, and its weight percent is that the distilled water liquid of 1wt% can play good dissemination to MWCNTs, and forms stable MWCNTs suspension.
According to bibliographical information ([1] Li Hongjian, Peng Jingcui, Chen Xiaohua, etc.The composite electromagnetic wave screened film of filling carbon nano-pipe/graphite, Chinese Journal of Chemical Physics, 2001,14 (2): 211-215; [2] Shen Cengmin, Yang Ziqin, Zhao Donglin, etc.The mechanical property of carbon nanotube/ABS resin based composites and the research of radar wave absorptive character, matrix material journal, 2003,20 (2): 25-29; [3] Wang Yimin, Ni Jianhua, Pan Xiangqing, etc.Gel-spun ultra-high molecular weight polyethylene/carbon nano tube composite fibre and preparation thereof, Chinese invention patent, application number 03115230.9; [4] Bertagna V, Delpeux S, JurewiczK, et al.Proceeding～Electrochemical Society, 2002,26 (Solid～State Ionic Devices III): 526-530; [5] Xiao Q F, Zhou X.Electrochimica Acta, 2003 (5), 48:575-580; Deng), estimate that the MWCNTs/SDS/PVA composite film material has good application prospects in following field: antistatic material, electrostatic spraying coating; The protecting materials of the read/write probe of computer; Water-soluble electromagnetic screen coating and wave-absorbing and camouflage coating; The fabric filamentary material, the protective clothing of special dimension and light, the comfortable flak jackets of dress; Ultracapacitor or electrochemical capacitor modulator material; Novel optical material etc.
Summary of the invention
The invention provides a kind of preparation method of MWCNTs/SDS/PVA composite film material, the preparation weight percent is the distilled water solution A of the polyvinyl alcohol (PVA) of 5～15wt%; The distilled water solution for preparing the sodium laurylsulfonate that weight percent is 1wt% (SDS) then, again purified multi-walled carbon nano-tubes (MWCNTs) sonic oscillation is dispersed in wherein, obtain MWCNTs suspension B, wherein the content of MWCNTs can be controlled in 0.1～1wt% scope; Distilled water solution A and the MWCNTs suspension B of PVA are mixed by a certain percentage; Obtain the mother solution C of MWCNTs content at the MWCNTs/SDS/PVA of 0.1～2wt% composite film material; With mother solution C striking film forming on clean, exsiccant glass film plates.The thickness of MWCNTs/SDS/PVA laminated film is between 28～100 microns.
Content 0.1～1wt%MWCNTs suspension B directly takes or re-uses after concentrating.
Described multi-walled carbon nano-tubes is to adopt the preparation of catalytic cracking methane method, and through air atmosphere oxidation and acid treatment two-step purifying, purity is greater than 98wt%.
The present invention is according to the preparation principle of general composite film material, and detailed step is:
(1) the PVA solid is added in the distilled water, be mixed with the water solution A that weight percent is the PVA of 5～15wt%.
(2) will adopt the MWCNTs crude product (Cui Lan etc., the method for nickel catalytic cracking methane preparing carbon nanometer tube, Chinese invention patent, ZL 00102824.3 for Cui Shen, Qiao Yali) of catalytic cracking methane method preparation to remove decolorizing carbon impurity in 2 hours 500 ℃ of heating; Re-use the 4M salpeter solution and handle 4h, remove catalyst impurities at 80 ℃ of following constant temperature; Use distilled water that filtration product is thoroughly washed then, reach neutral to the upper strata clear liquid; Filtration product is carried out finish-drying, promptly obtain the MWCNTs of purity greater than 98wt%.
(3) SDS is dissolved in the distilled water, the preparation weight percent is the distilled water solution of the SDS of 1wt%, more purified MWCNTs sonic oscillation is dispersed in wherein, and obtaining weight percent is the stable MWCNTs suspension B of 0.1～1wt%.
(4) the distilled water solution A of the PVA of 5～15wt% and the stable MWCNTs suspension B of 0.1～1wt% are mixed by a certain percentage, obtain the mother solution C of the MWCNTs/SDS/PVA composite film material of MWCNTs content between 0.1～2wt%.
(5) with the solution scrub of glass film plates ethanol: ether=1:1, dry leveling; Parallel tying up at a distance of 15 centimetres of intervals, the copper enameled wire (controlling film forming thickness) of diameter between 30～110 microns; Under dustproof environment, above-mentioned mother solution C evenly is poured on the glass film plates, with special scraper along parallel copper enameled wire blade coating film forming, drying at room temperature 24 hours; Vacuum constant temperature is dry 3 hours then.
(6) the above-mentioned glass film plates that is loaded with laminated film is immersed in the distilled water, take off film, dry, promptly obtain the MWCNTs/SDS/PVA laminated film of thickness between 28～100 microns.
The present invention has following advantage:
(1) the MWCNTs crude product of the present invention's use is to adopt the preparation of catalytic cracking methane method, and cost is lower;
(2) used primary solvent is a distilled water, environmentally safe;
(3) the MWCNTs/SDS/PVA laminated film is nontoxic substantially, harmless, pollution-free to environment;
(4) the MWCNTs/SDS/PVA laminated film not only is being significantly improved aspect mechanics, the electric property, aspect thermostability be improved significantly, permeability also improves, and the stability of (liquid nitrogen temperature) is greatly improved under ultra-low temperature surroundings;
(5) the MWCNTs/SDS/PVA laminated film is at antistatic material, electrostatic spraying coating, water-soluble electromagnetic screen coating and wave-absorbing and camouflage coating, the fabric filamentary material, the protective clothing of special dimension or wear light, comfortable flak jackets, ultracapacitor or electrochemical capacitor modulator material, there is good application prospects in fields such as novel optical material;
(6) the present invention not only is applicable to the preparation of MWCNTs/SDS/PVA laminated film, also is applicable to the preparation of the laminated film of all water-soluble polymerss and MWCNTs/SDS.
Embodiment
Embodiment 1
(1) takes by weighing 10 gram PVA solids, slowly add in the 90 gram distilled water that stirring, be heated to 93 ℃ gradually, continue to be stirred to PVA and dissolve fully, be cooled to room temperature then; Get the supernatant liquid of filtrate after the filtration, standing and defoaming 24 hours; Obtain the water solution A that weight percent is about the PVA of 10wt%.
(2) take by weighing MWCNTs crude product 1 gram that the catalytic cracking methane method prepares, at 450～500 ℃ of heating 2 hours, the about 20wt% of rate of weight loss.Above-mentioned about 0.8 gram of handling through calcination of MWCNTs sample is placed 100 milliliters of 4M salpeter solutions,, be cooled to room temperature 80 ℃ of constant temperature 4 hours; Filter, with distilled water precipitation is washed then, reach neutral to filtrate; Final filtration product is carried out finish-drying, promptly obtain the MWCNTs of purifying, purity is greater than 98wt%; The about 90wt% of purification yield.
(3) 0.995 gram SDS is dissolved in the 98.505 gram distilled water, make the distilled water solution that weight percent is the SDS of 1wt%, purified 0.5 gram MWCNTs is added wherein, sonic oscillation disperseed 0.5 hour again, and obtaining weight percent is the stable MWCNTs suspension B of 0.5wt%.
(4) the suspension B of the stable MWCNTs of the 0.5wt% that the distilled water solution A and 10 of the PVA of the 10wt% of 40 grams is restrained mixes, and obtains the mother solution C of 0.1wt%MWCNTs/0.2wt%SDS/PVA composite film material.
(5) with the solution scrub of glass film plates ethanol: ether=1:1, dry horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire (controlling film forming thickness) of 30 microns of diameters; Under dustproof environment, above-mentioned mother solution C evenly is poured on the glass film plates, with special scraper along parallel copper enameled wire blade coating film forming, drying at room temperature 24 hours; Freeze-day with constant temperature 3 hours under vacuum, 110 ℃ of conditions then.
(6) will be loaded with in the glass film plates immersion distilled water of laminated film, take off film, dry, promptly obtain the about 28 microns 0.1wt%MWCNTs/0.2wt%SDS/PVA laminated film of thickness.
Adopt stretching method to measure the mechanical property of MWCNTs/SDS/PVA laminated film; Mechanical meaurement is the result show, the breaking tenacity of 0.1wt%MWCNTs/0.2wt%SDS/PVA laminated film is 56 MPas (MPa).Adopt the two electrodes method to measure the volume specific resistance of MWCNTs/SDS/PVA laminated film; Electrical measurement is the result show, the volume specific resistance of 0.1wt%MWCNTs/0.2wt%SDS/PVA laminated film is 2.7 * 10
13Ohm meter (Ω m).
Embodiment 2
Solution scrub with glass film plates ethanol: ether=1:1 dries horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire of 44 microns of diameters, other experiment condition obtains the about 40 microns 0.1wt%MWCNTs/0.2wt%SDS/PVA laminated film of thickness with embodiment 1.
Mechanical meaurement is the result show, its breaking tenacity is about 64MPa, Young's modulus 1.85 gpa (GPa).Electrical measurement is the result show, its volume specific resistance is 2.2 * 10
13Ω m.The thermogravimetric measuring result shows, is 18wt% at the rate of weight loss below 300 ℃, and the rate of weight loss in 320 ℃～480 ℃ of intervals is 78wt%; Be heated to 700 ℃, total rate of weight loss 93wt%.The hydrogen permeate coefficient of this laminated film is 2.61molcm/mincm
2KPa.This laminated film print bar (long 80 millimeters, wide 15 millimeters, down together) in liquid nitrogen, place after 15 minutes, brittle rupture takes place when crooked under external force.
Embodiment 3
Solution scrub with glass film plates ethanol: ether=1:1 dries horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire of 56 microns of diameters, other experiment condition obtains the about 50 microns 0.1wt%MWCNTs/0.2wt%SDS/PVA laminated film of thickness with embodiment 1.
Mechanical meaurement is the result show, its breaking tenacity is about 70MPa.Electrical measurement is the result show, its volume specific resistance is 2.1 * 10
13Ω m.
Embodiment 4
The stable MWCNTs suspension B of the 0.5wt% that the distilled water solution A and 25 of the PVA of the 10wt% of 25 grams is restrained mixes, other experiment condition obtains the about 40 microns 0.25wt%MWCNTs/0.5wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 72MPa, Young's modulus 1.90GPa.Electrical measurement is the result show, its volume specific resistance is 1.0 * 10
13Ω m.The hydrogen permeate coefficient of this laminated film is 2.42molcm/mincm
2KPa.This laminated film sample strip is placed 15 minutes in liquid nitrogen after, when crooked under external force brittle rupture can not take place; Sample strip continues to place (accumulative total 30 minutes) after 15 minutes in liquid nitrogen, brittle rupture takes place when crooked under external force.
Embodiment 5
The suspension B of the stable MWCNTs of the 1wt% that the distilled water solution A and 25 of the PVA of the 10wt% of 25 grams is restrained mixes, other experiment condition obtains the about 40 microns 0.5wt%MWCNTs/0.5wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 78MPa, Young's modulus 1.97GPa.Electrical measurement is the result show, its volume specific resistance is 1.2 * 10
12Ω m.The thermogravimetric measuring result shows, is 15wt% at the rate of weight loss below 300 ℃, and the rate of weight loss in 320 ℃～480 ℃ of intervals is 77wt%; Be heated to 700 ℃, total rate of weight loss 92wt%.The hydrogen permeate coefficient of this laminated film is 2.40molcm/mincm
2KPa.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, still brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 6
The suspension B heating that takes by weighing the stable MWCNTs of 50 1wt% that restrain is concentrated into 25 grams, the distilled water solution A of PVA with the 10wt% of 25 grams mixes again, other experiment condition obtains the about 28 microns 1.0wt%MWCNTs/1.0wt%SDS/PVA laminated film of thickness with embodiment 1.
Mechanical meaurement is the result show, its breaking tenacity is about 70MPa.Electrical measurement is the result show, its volume specific resistance is 2.3 * 10
12Ω m.
Embodiment 7
The blending ratio of stable MWCNTs suspension B and the distilled water solution A of PVA is with embodiment 6, and other experiment condition obtains the about 40 microns 1.0wt%MWCNTs/1.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 80MPa, Young's modulus 2.64GPa.Electrical measurement is the result show, its volume specific resistance is 3.3 * 10
11Ω m.The hydrogen permeate coefficient of this laminated film is 2.36molcm/mincm
2KPa.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, also brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 8
The blending ratio of stable MWCNTs suspension B and the distilled water solution A of PVA is with embodiment 6, and other experiment condition obtains the about 50 microns 1.0wt%MWCNTs/1.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 3.
Mechanical meaurement is the result show, its breaking tenacity is about 84MPa.Electrical measurement is the result show, its volume specific resistance is 2.0 * 10
11Ω m.
Embodiment 9
Solution scrub with glass film plates ethanol: ether=1:1 dries horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire of 110 microns of diameters, other experiment condition obtains the about 100 microns 1.0wt%MWCNTs/1.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 6.
Mechanical meaurement is the result show, its breaking tenacity is about 90MPa.Electrical measurement is the result show, its volume specific resistance is 6.1 * 10
10Ω m.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, also brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 10
The stable MWCNTs suspension B heating that takes by weighing the 1wt% of 100 grams is concentrated into 25 grams, the distilled water solution A of PVA with the 10wt% of 25 grams mixes again, other experiment condition obtains the about 40 microns 2.0wt%MWCNTs/2.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 82MPa, Young's modulus 2.69GPa.Electrical measurement is the result show, its volume specific resistance is 1.7 * 10
11Ω m.The thermogravimetric measuring result shows, is 11wt% at the rate of weight loss below 300 ℃, and the rate of weight loss in 320 ℃～480 ℃ of intervals is 78wt%; Be heated to 700 ℃, total rate of weight loss 92wt%.The hydrogen permeate coefficient of this laminated film is 2.10molcm/mincm
2KPa.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, also brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 11
With reference to the step among the embodiment 1 (1), the distilled water solution A of the PVA of the 5wt% of preparation 25 grams; The stable MWCNTs suspension B heating that takes by weighing the 1wt% of 100 grams is concentrated into 25 grams, the distilled water solution A of PVA with the 5wt% of 25 grams mixes again, other experiment condition obtains the about 40 microns 2.0wt%MWCNTs/2.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 78MPa.Electrical measurement is the result show, its volume specific resistance is 1.6 * 10
11Ω m.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, also brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 12
With reference to the step among the embodiment 1 (1), the distilled water solution A of the PVA of the 15wt% of preparation 25 grams; The suspension B heating that takes by weighing the stable MWCNTs of 100 1wt% that restrain is concentrated into 25 grams, the distilled water solution A of PVA with the 15wt% of 25 grams mixes again, other experiment condition obtains the about 40 microns 2.0wt%MWCNTs/2.0wt%SDS/PVA laminated film of thickness with embodiment 1 and embodiment 2.
Mechanical meaurement is the result show, its breaking tenacity is about 76MPa.Electrical measurement is the result show, its volume specific resistance is 1.8 * 10
11Ω m.This laminated film sample strip is placed 60 minutes in liquid nitrogen after, also brittle rupture can not take place when crooked under external force, i.e. crooked 180 degree of sample strip are cancelled after the external force still resilient.
Embodiment 13
0.4975 gram SDS is dissolved in the 49.2525 gram distilled water, make the distilled water solution that weight percent is the SDS of 1wt%, again purified 0.05 gram MWCNTs is added wherein, sonic oscillation disperseed 0.5 hour, obtaining weight percent is the stable MWCNTs suspension B of 0.1wt%, heating is concentrated into 24.9 grams, and the distilled water solution A of PVA with the 10wt% of 24.9 grams mixes again; Other experiment condition obtains the about 28 microns 0.1wt%MWCNTs/1.0wt%SDS/PVA laminated film of thickness with embodiment 1.
Mechanical meaurement is the result show, its breaking tenacity is about 54MPa.
Embodiment 14
0.5 gram SDS is dissolved in the 24.5 gram distilled water, makes the distilled water solution that weight percent is the SDS of 2wt%; The distilled water solution A of PVA with the 10wt% of itself and 25 grams mixes again, and obtaining SDS content is the mother solution C of the SDS/PVA composite film material of 1wt%.Other experiment condition obtains the about 28 microns 1wt%SDS/PVA laminated film of thickness with Comparative Examples 1.
Mechanical meaurement is the result show, the breaking tenacity of this 1wt%SDS/PVA laminated film is 53MPa.This laminated film print bar is placed 15 minutes in liquid nitrogen after, brittle rupture takes place when crooked under external force.
Embodiment 15
Solution scrub with glass film plates ethanol: ether=1:1 dries horizontal positioned; Parallelly on glass film plates tie up at a distance of, 15 centimetres of intervals, the copper enameled wire of 44 microns of diameters, other experiment condition obtains the about 40 microns 1wt%SDS/PVA laminated film of thickness with Comparative Examples 1 and embodiment 14.
Mechanical meaurement is the result show, its breaking tenacity is about 57MPa, Young's modulus 1.63GPa.The hydrogen permeate coefficient of this laminated film is 3.37molcm/mincm
2KPa.This laminated film sample strip is placed 15 minutes in liquid nitrogen after, brittle rupture takes place when crooked under external force.
Comparative Examples 1
(1) takes by weighing 10 gram PVA solids, slowly add in the 90 gram distilled water that stirring, be heated to 93 ℃ gradually, continue to be stirred to PVA and dissolve fully, be cooled to room temperature then; Get the supernatant liquid of filtrate after the filtration, standing and defoaming 24 hours; Obtain the water solution A that weight percent is about the PVA of 10wt%.
(2) with the solution scrub of glass film plates ethanol: ether=1:1, dry horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire of 30 microns of diameters; Under dustproof environment, above-mentioned water solution A evenly is poured on the glass film plates, with special scraper along parallel copper enameled wire blade coating film forming, drying at room temperature 24 hours; Freeze-day with constant temperature 3 hours under vacuum, 110 ℃ of conditions then.
(3) will be loaded with in the glass film plates immersion distilled water of PVA film, take off film, dry, promptly obtain the about 28 microns PVA film of thickness.
Mechanical meaurement is the result show, the breaking tenacity of this PVA film is 56MPa.Electrical measurement is the result show, the volume specific resistance of this PVA film is 3.2 * 10
13Ω m.This PVA film print bar is placed 15 minutes in liquid nitrogen after, brittle rupture takes place when crooked under external force.
Comparative Examples 2
Solution scrub with glass film plates ethanol: ether=1:1 dries horizontal positioned; Parallelly on glass film plates tie up at a distance of 15 centimetres of intervals, the copper enameled wire of 44 microns of diameters, other experiment condition obtains the about 40 microns PVA film of thickness with Comparative Examples 1.
Mechanical meaurement is the result show, its breaking tenacity is about 60MPa, Young's modulus 1.72GPa.Electrical measurement is the result show, its volume specific resistance is 3.1 * 10
13Ω m.The thermogravimetric measuring result shows, is 20wt% at the rate of weight loss below 300 ℃, and the rate of weight loss in 320 ℃～480 ℃ of intervals is 70wt%; Be heated to 700 ℃, total rate of weight loss 95wt%.The hydrogen permeate coefficient of this PVA film is 3.11molcm/mincm
2KPa.This PVA film sample bar is placed 15 minutes in liquid nitrogen after, brittle rupture takes place when crooked under external force.
The preparation method of multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film that the present invention proposes, be described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to device as herein described with technological method is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (4)
1. the preparation method of a multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film is characterized in that preparing the distilled water solution A of the polyvinyl alcohol that weight percent is 5～15wt% (PVA); The distilled water solution for preparing the sodium laurylsulfonate that weight percent is 1wt% (SDS) then, again purified multi-walled carbon nano-tubes (MWCNTs) sonic oscillation is dispersed in wherein, obtain MWCNTs suspension B, wherein the content of MWCNTs is in 0.1～1wt% scope; Solution A and suspension B mix, and obtain the mother solution C of MWC NTs content at the MWCNTs/SDS/PVA of 0.1～2wt% composite film material; With mother solution C striking film forming on clean, exsiccant glass film plates.
2. the preparation method of multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film as claimed in claim 1 is characterized in that content 0.1～1wt%MWCNTs suspension B directly takes or re-uses after concentrating.
3. the preparation method of multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film as claimed in claim 1, it is characterized in that described multi-walled carbon nano-tubes is to adopt the preparation of catalytic cracking methane method, and through air atmosphere oxidation and acid treatment two-step purifying, purity is greater than 98wt%.
4. the preparation method of multi-wall carbon nano-tube/dodecyl sodium sulfonate sodium/polyvinyl alcohol compound film as claimed in claim 1,, the thickness that it is characterized in that the MWCNTs/SDS/PVA laminated film is between 28～100 microns.
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| CN102139189A (en) * | 2011-01-25 | 2011-08-03 | 哈尔滨工业大学（威海） | Method for preparing seawater desalting electro-filtration ionic membrane |
| CN102660097B (en) * | 2012-04-11 | 2013-07-10 | 上海交通大学 | Preparation method of reinforced polyvinyl alcohol compound |
| CN102660097A (en) * | 2012-04-11 | 2012-09-12 | 上海交通大学 | Preparation method of reinforced polyvinyl alcohol compound |
| CN103173003B (en) * | 2013-02-27 | 2015-05-20 | 国家纳米科学中心 | Carbon nanotube-water-soluble polymer composite flexible electric-heating film as well as preparation method and use thereof |
| CN103173003A (en) * | 2013-02-27 | 2013-06-26 | 国家纳米科学中心 | Carbon nanotube-water-soluble polymer composite flexible electric-heating film as well as preparation method and use thereof |
| CN103521276A (en) * | 2013-10-12 | 2014-01-22 | 东华大学 | Carbon-nanotube-doped type basic anion exchange composite membrane, and preparation method and application thereof |
| CN103521276B (en) * | 2013-10-12 | 2016-01-20 | 东华大学 | A kind of carbon nano tube-doped type alkaline negative ion exchange composite film and its preparation method and application |
| CN103603140A (en) * | 2013-11-20 | 2014-02-26 | 东华大学 | Preparation method of composite nanofiber material |
| CN103603140B (en) * | 2013-11-20 | 2016-11-23 | 东华大学 | A kind of preparation method of composite nano-fiber material |
| CN110898801A (en) * | 2019-07-29 | 2020-03-24 | 武汉理工大学 | Preparation of carbon nano tube and sludge biochar composite material and application of composite material in removing low-concentration sulfamethoxazole in water |
| CN110556559A (en) * | 2019-09-16 | 2019-12-10 | 东北大学 | Method for preparing low-temperature proton exchange membrane with layered structure based on vacuum-assisted flocculation technology |
| CN110556559B (en) * | 2019-09-16 | 2022-06-14 | 东北大学 | Method for preparing low-temperature proton exchange membrane with layered structure based on vacuum-assisted flocculation technology |
| CN117362913A (en) * | 2023-10-24 | 2024-01-09 | 山东莱芜润达新材料有限公司 | Thermoplastic phenolic resin and granulating process thereof |
| CN117362913B (en) * | 2023-10-24 | 2024-04-16 | 山东莱芜润达新材料有限公司 | Thermoplastic phenolic resin and granulating process thereof |
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