CN103147355A - Preparation method of biomass nano fiber conductive paper - Google Patents
Preparation method of biomass nano fiber conductive paper Download PDFInfo
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- CN103147355A CN103147355A CN2013100594522A CN201310059452A CN103147355A CN 103147355 A CN103147355 A CN 103147355A CN 2013100594522 A CN2013100594522 A CN 2013100594522A CN 201310059452 A CN201310059452 A CN 201310059452A CN 103147355 A CN103147355 A CN 103147355A
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Abstract
The invention discloses a preparation method of biomass nano fiber conductive paper. High-conductivity carbon nanotubes are added into a viscous nano fiber/cellulose thickening agent mixed solution, and high-speed homogenization is utilized to mechanically shear the outer layer structure of the carbon nanotubes, so that the carbon nanotubes have polarity and can be combined with hydroxy groups on the cellulose nano fibril fiber surface; and meanwhile, by the aid of the aggregation of the high-viscosity retardant carbon nanotubes of the nano fiber/cellulose thickening agent solution, the nano fiber/cellulose thickening agent solution can be uniformly and stably dispersed. The preparation method of biomass cellulose conductive paper has the advantages of simple and controllable production process, environmental protection and appropriate cost; and meanwhile, the large-specific-area cellulose nano fibril in a natural network structure can adsorb and combine more carbon nanotubes, and the composite conductive paper has the advantages of low resistance, stable conductivity, high mechanical strength and high heat stability, and can be widely used in the fields of multidimensional conductive materials, unconventional conductive materials, multifunctional energy storage materials, novel electromagnetic shielding and electromagnetic sensing materials and the like.
Description
Technical field
The present invention relates to the preparation method of biomass nano Conductivity of Fiber electric material, be specially a kind of preparation method of biomass nano fiber conductive paper.
Background technology
The string conductive paper not only has good conduction and effectiveness, also has aboundresources, ecological, environmental protective, and the advantage such as with low cost is gaining great popularity as a kind of novel conductive material in recent years.Yet string itself can not conduct electricity, and needs to introduce conducting polymer or inorganic conductive material etc. compound with it, builds the charge-conduction latus rectum, realizes the conducting function of string.CNT (single wall or many walls) has excellent electric conductivity and natural network structure, can create the high-effective conductive latus rectum, has become the optimal material of preparation string conductive paper.And in the preparation process of this string conductive paper, dissolving each other and effectively combination of string and DIC nanotube is the key factor that determines material property.Adopt the cellulose of ionic liquid at room temperature dissolving, can mix with the CNT interworking, but the removing of its unnecessary ionic liquid and residue thereof is still complicated loaded down with trivial details, utilization by the surfactants such as mersolates, methylmorphine can be in water effective dispersing Nano carbon tubes, but the dispersion process program is complicated, poor controllability, and some dispersant is to environment and ecological harmful simultaneously.
The cellulose nanofibrils often utilizes the method for high speed machine shearing or chemical oxidation as the important biomass nano fibrous material of a class, the cellulose microfibril in string is separated disassemble into diameter in the elongated fibers of nanoscale (lower than 100nm).Not only mechanical property is strong for it, draw ratio is high, can also be stable colloidal in the aqueous solution.Utilize suitable method Uniform Dispersion CNT in nanofiber solution, can not only obtain mechanical strength high, the conductive nano paper material of good conductivity, the nanometer small size of material and quantum effect can also give material new electromagnetic property.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation method of biomass nano fiber conductive paper, to solve the shortcoming in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of preparation method of biomass nano fiber conductive paper, the distinguishing feature that is different from other technique utilize the layer structure of high speed homogenization mechanical shearing destroying carbon nanometer tube, make it present polarity, with cellulose nanofibrils fiber surface hydroxy combining.Utilize simultaneously the reunion of the high viscosity retardance CNT of nanofiber mixed solution, make its uniform and stable dispersion.Then adopt excessive moisture in the method elimination mixed solution that is similar to traditional papermaking, obtain the biomass nano fiber conductive paper composite of excellent performance, comprise the following steps:
The 1st step: the thickener hydroxypropyl methylcellulose is dissolved in cellulose nanofibrils solution, and thickener qualities accounts for the 3-5% of mixed material (dry state).Add deionized water that above-mentioned mixed solution is diluted to 0.2-0.3wt% under the high-speed stirred condition.
The 2nd step: a certain amount of CNT is added in the mixed solution of diluted state cellulose nanofibrils and thickener the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
The 3rd step: the high speed homogenization mechanical shearing is processed.Shear dispersion treatment through the preliminary mixed solution that disperses in the microjet high pressure homogenizer, wherein the reaction chamber of 200 μ m and 87 μ m is united use, and circulation shear is processed 5-8 time.
The 4th step: the carbon nanotube/nano fiber mixed solution through fully disperseing is elimination part moisture in pressurization (or vacuum) filtration system, forms the colloidal wet film.Wet film under the plus load condition through Adsorption of Filter Paper excessive moisture, heat drying to over dry.
In the present invention, in described the 1st step, thickener can be hydroxypropyl methylcellulose, hydroxyethylcellulose, carboxy methyl cellulose, perhaps their mixture, but the addition of thickener need be controlled at 3-5wt%, regulates according to the viscosity of raw cellulose nanofibrils solution.
In the present invention, add the cellulose nanofibrils mixed solution after thickener need regulate solid content to 0.2-0.3% in described the 1st step, in follow-up high speed shear process, material stops up in reaction chamber to avoid.
In the present invention, in described the 2nd step, addition depending on the target material of CNT require, and general addition is that 3-6wt% gets final product, and can not surpass 15wt% at most.
In the present invention, in described the 3rd step during microjet high pressure homogenizer shear treatment, in 200-87 μ m association response chamber, pressure is 140-160MPa.
In the present invention, in described the 3rd step, during microjet high pressure homogenizer shear treatment, the circulation shear number of times is 4-8 time.
In the present invention, in described the 4th step, carbon nanotube/nano fiber mixed solution need filter through the cellulose permeable membrane, and wherein the aperture of filter membrane is 0.2-0.7 μ m.
In the present invention, in described the 4th step, the wet film dry run need apply external pressure and prevent its contraction distortion.In order to guarantee that in conductive paper, moisture is removed fully, can be under 100-105 ℃ of heating condition further dry 1h.
Beneficial effect: the preparation method of biomass nano fiber conductive paper of the present invention utilizes the layer structure of high speed homogenization mechanical shearing destroying carbon nanometer tube, makes it present polarity, can with cellulose nanofibrils fiber surface hydroxy combining.Block simultaneously the reunion of CNT by the high viscosity of nanofiber/cellulose thickener solution, make its uniform and stable dispersion.The cellulose conductive paper production process that obtains by this method is simple and easy to control, environmental protection, cost are suitable.Simultaneously, bigger serface, natural cancellated cellulose nanofibrils can adsorb, the more CNT of combination, composite conducting paper overall performance is better than traditional micron order string conductive paper, can be applicable to the fields such as unconventional conductive material, energy storage material, novel electromagnetic shielding and sensing material.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
The 1st step: the thickener hydroxypropyl methylcellulose is dissolved in cellulose nanofibrils solution, and thickener qualities accounts for 3% of mixed material (dry state).In follow-up high speed shear process, material stops up in reaction chamber in order to avoid, and adds deionized water that above-mentioned mixed solution is diluted to 0.2wt% under stirring condition.
The 2nd step: the CNT of 5wt% is added in the cellulose nanofibrils of diluted state/hydroxypropyl methylcellulose mixed solution the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
The 3rd step: the high speed homogenization mechanical shearing is processed.Shear dispersion treatment through the preliminary mixed solution that disperses in the microjet high pressure homogenizer, wherein the reaction chamber of 200 μ m and 87 μ m is united use, and reaction pressure is 150MPa, and circulation shear is processed 6 times.
The 4th step: the carbon nanotube/nano fiber mixed solution through fully disperseing through the cellulose filter paper elimination part moisture in 0.2 μ m aperture, forms the colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under the 500N plus load, then under 100-105 ℃ of heating condition further dry 1h.
Embodiment 2
The 1st step: the thickener hydroxypropyl methylcellulose is dissolved in cellulose nanofibrils solution, and thickener qualities accounts for 4% of mixed material (dry state).In follow-up high speed shear process, material stops up in reaction chamber in order to avoid, and adds deionized water that above-mentioned mixed solution is diluted to 0.3wt% under stirring condition.
The 2nd step: the CNT of 6wt% is added in the cellulose nanofibrils of diluted state/hydroxypropyl methylcellulose mixed solution the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
The 3rd step: the high speed homogenization mechanical shearing is processed.Shear dispersion treatment through the preliminary mixed solution that disperses in the microjet high pressure homogenizer, wherein the reaction chamber of 200 μ m and 87 μ m is united use, and reaction pressure is 150MPa, and circulation shear is processed 8 times.
The 4th step: the carbon nanotube/nano fiber mixed solution through fully disperseing through the cellulose filter paper elimination part moisture in 0.4 μ m aperture, forms the colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under the 500N plus load, then under 100-105 ℃ of heating condition further dry 1h.
Embodiment 3
The 1st step: the thickener hydroxypropyl methylcellulose is dissolved in cellulose nanofibrils solution, and thickener qualities accounts for 5% of mixed material (dry state).In follow-up high speed shear process, material stops up in reaction chamber in order to avoid, and adds deionized water that above-mentioned mixed solution is diluted to 0.2wt% under stirring condition.
The 2nd step: the CNT of 7wt% is added in the cellulose nanofibrils of diluted state/hydroxypropyl methylcellulose mixed solution the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
The 3rd step: the high speed homogenization mechanical shearing is processed.Shear dispersion treatment through the preliminary mixed solution that disperses in the microjet high pressure homogenizer, wherein the reaction chamber of 200 μ m and 87 μ m is united use, and reaction pressure is 150MPa, and circulation shear is processed 8 times.
The 4th step: the carbon nanotube/nano fiber mixed solution through fully disperseing through the cellulose filter paper elimination part moisture in 0.5 μ m aperture, forms the colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under the 500N plus load, then under 100-105 ℃ of heating condition further dry 1h.
Above demonstration and described basic principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and the claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (8)
1. the preparation method of a biomass nano fiber conductive paper, its characteristics are, comprise the following steps:
The 1st step: the thickener hydroxypropyl methylcellulose is dissolved in cellulose nanofibrils solution, and thickener qualities accounts for the 3-5% of the mixed material of dry state, adds deionized water that above-mentioned mixed solution is diluted to 0.2-0.3wt% under the high-speed stirred condition;
The 2nd step: a certain amount of CNT is added in the mixed solution of diluted state cellulose nanofibrils and thickener the preliminary dispersing Nano carbon tubes of mechanical agitation 10min;
The 3rd step: the high speed homogenization mechanical shearing is processed, and shears dispersion treatment through the preliminary mixed solution that disperses in the microjet high pressure homogenizer, and wherein the reaction chamber of 200 μ m and 87 μ m is united use, and circulation shear is processed 5-8 time;
The 4th step: the carbon nanotube/nano fiber mixed solution through fully disperseing is elimination part moisture in pressurization (or vacuum) filtration system, forms the colloidal wet film, wet film under the plus load condition through Adsorption of Filter Paper excessive moisture, heat drying to over dry.
2. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, it is characterized in that, in described the 1st step, thickener can be hydroxypropyl methylcellulose, hydroxyethylcellulose, carboxy methyl cellulose, perhaps their mixture, but the addition of thickener need be controlled at 3-5wt%, regulates according to the viscosity of raw cellulose nanofibrils solution.
3. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, it is characterized in that, add the cellulose nanofibrils mixed solution after thickener need regulate solid content to 0.2-0.3% in described the 1st step, in follow-up high speed shear process, material stops up in reaction chamber to avoid.
4. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described the 2nd step, addition depending on the target material of CNT require, and general addition is that 3-6wt% gets final product, and can not surpass 15wt% at most.
5. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described the 3rd step during microjet high pressure homogenizer shear treatment, in 200-87 μ m association response chamber, pressure is 140-160MPa.
6. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described the 3rd step, during microjet high pressure homogenizer shear treatment, the circulation shear number of times is 4-8 time.
7. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described the 4th step, carbon nanotube/nano fiber mixed solution need filter through the cellulose permeable membrane, and wherein the aperture of filter membrane is 0.2-0.7 μ m.
8. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, it is characterized in that, in described the 4th step, the wet film dry run need apply external pressure and prevent its contraction distortion, in order to guarantee that in conductive paper, moisture is removed fully, can be under 100-105 ℃ of heating condition further dry 1h.
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| WO2015057168A1 (en) * | 2013-10-17 | 2015-04-23 | Nanyang Technological University | Conductive paper and method of forming the same |
| CN104674582A (en) * | 2013-12-03 | 2015-06-03 | 金东纸业（江苏）股份有限公司 | Pulp, preparation method of pulp, and paper made of pulp |
| CN107201689A (en) * | 2017-06-01 | 2017-09-26 | 大连理工大学 | A kind of preparation method of carbon nano tube electromagnetic shielding paper |
| CN109799012A (en) * | 2019-01-23 | 2019-05-24 | 河南工程学院 | A kind of class sandwich structure pressure sensor and preparation method thereof based on cellulose |
| CN109796007A (en) * | 2019-02-19 | 2019-05-24 | 昆明理工大学 | Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube |
| CN110157393A (en) * | 2019-05-06 | 2019-08-23 | 滨州学院 | Drilling fluid proposes viscous extracting and cutting agent and preparation method with nanofiber-xanthan gum compound |
| US10435571B2 (en) | 2014-05-22 | 2019-10-08 | Lg Chem, Ltd. | Method for preparing carbon nanotube, and dispersion composition of carbon nanotube |
| CN110317441A (en) * | 2019-06-26 | 2019-10-11 | 浙江理工大学 | A kind of preparation method of high-intensity high every property polylactic acid base nano compound film |
| CN111945460A (en) * | 2020-07-31 | 2020-11-17 | 齐鲁工业大学 | Method for dispersing short carbon fibers and application |
| CN113881108A (en) * | 2021-10-07 | 2022-01-04 | 华南理工大学 | Pineapple leaf fiber-reinforced flexible electromagnetic shielding film and preparation method thereof |
| CN115819848A (en) * | 2022-11-28 | 2023-03-21 | 浙江大学 | Multifunctional nano-cellulose composite solution and preparation method and application thereof |
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Cited By (17)
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| WO2015057168A1 (en) * | 2013-10-17 | 2015-04-23 | Nanyang Technological University | Conductive paper and method of forming the same |
| CN104674582A (en) * | 2013-12-03 | 2015-06-03 | 金东纸业（江苏）股份有限公司 | Pulp, preparation method of pulp, and paper made of pulp |
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| US10435571B2 (en) | 2014-05-22 | 2019-10-08 | Lg Chem, Ltd. | Method for preparing carbon nanotube, and dispersion composition of carbon nanotube |
| CN107201689A (en) * | 2017-06-01 | 2017-09-26 | 大连理工大学 | A kind of preparation method of carbon nano tube electromagnetic shielding paper |
| CN107201689B (en) * | 2017-06-01 | 2019-03-26 | 大连理工大学 | A kind of preparation method of carbon nano tube electromagnetic shielding paper |
| CN109799012A (en) * | 2019-01-23 | 2019-05-24 | 河南工程学院 | A kind of class sandwich structure pressure sensor and preparation method thereof based on cellulose |
| CN109799012B (en) * | 2019-01-23 | 2021-01-22 | 河南工程学院 | Cellulose-based sandwich-like structure pressure sensor and preparation method thereof |
| CN109796007A (en) * | 2019-02-19 | 2019-05-24 | 昆明理工大学 | Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube |
| CN109796007B (en) * | 2019-02-19 | 2022-03-15 | 昆明理工大学 | Preparation method of micro-nano biomass fiber and carbon nanotube mixed suspension |
| CN110157393A (en) * | 2019-05-06 | 2019-08-23 | 滨州学院 | Drilling fluid proposes viscous extracting and cutting agent and preparation method with nanofiber-xanthan gum compound |
| CN110317441A (en) * | 2019-06-26 | 2019-10-11 | 浙江理工大学 | A kind of preparation method of high-intensity high every property polylactic acid base nano compound film |
| CN111945460A (en) * | 2020-07-31 | 2020-11-17 | 齐鲁工业大学 | Method for dispersing short carbon fibers and application |
| CN113881108A (en) * | 2021-10-07 | 2022-01-04 | 华南理工大学 | Pineapple leaf fiber-reinforced flexible electromagnetic shielding film and preparation method thereof |
| CN115819848A (en) * | 2022-11-28 | 2023-03-21 | 浙江大学 | Multifunctional nano-cellulose composite solution and preparation method and application thereof |
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