CN103147355B - A kind of preparation method of biomass nano fiber conductive paper - Google Patents
A kind of preparation method of biomass nano fiber conductive paper Download PDFInfo
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- CN103147355B CN103147355B CN201310059452.2A CN201310059452A CN103147355B CN 103147355 B CN103147355 B CN 103147355B CN 201310059452 A CN201310059452 A CN 201310059452A CN 103147355 B CN103147355 B CN 103147355B
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Abstract
The invention discloses a kind of preparation method of biomass nano fiber conductive paper, high conductivity CNT adds in viscosity nanofiber/cellulose thickener mixed solution by it, utilize the layer structure of high speed homogenisation mechanical shearing bad CNT, it is made to present polarity, with cellulose nanometer fibril fiber surface hydroxy combining.Simultaneously by the reunion of the high viscosity retardance CNT of nanofiber/cellulose thickener solution, make its uniform and stable dispersion.The biomass cellulose conductive paper production process obtained by this method is simple and easy to control, environmental protection, cost are suitable.Simultaneously, bigger serface, natural cancellated cellulose nanometer fibril can be adsorbed, in conjunction with more CNT, composite conductive paper impedance is low, stable conductivity, mechanical strength are high, Heat stability is good, can be widely used in the various fields such as multidimensional conductive material, unconventional conductive material, multifunction energy storage material, novel electromagnetic shielding and electromagnetic sensing material.
Description
Technical field
The present invention relates to the preparation method of biomass nano fibrous conductive material, be specially a kind of preparation method of biomass nano fiber conductive paper.
Background technology
The advantages such as string conductive paper not only has good conduction and effectiveness, also has aboundresources, ecological, environmental protective, with low cost, are gaining great popularity as a kind of novel conductive material in recent years.But string itself can not conduct electricity, need to introduce conducting polymer or inorganic conductive material etc. and its compound, build charge-conduction latus rectum, realize the conducting function of string.CNT (single wall or many walls) has excellent electric conductivity and natural network structure, can create high-effective conductive latus rectum, become the optimal material preparing string conductive paper.And in the preparation process of this string conductive paper, string dissolves each other with DIC nanotube and is effectively combined, it is the key factor determining material property.Adopt the cellulose that ionic liquid at room temperature dissolves, can mix with CNT interworking, but the removing of its excess ions liquid and residue thereof is still complicated loaded down with trivial details, utilize by the surfactant such as mersolates, methylmorphine can in water effective dispersing Nano carbon tubes, but dispersion process program is complicated, poor controllability, some dispersant is harmful to environment and ecology simultaneously.
Cellulose nanometer fibril, as the important biomass nano fibrous material of a class, often utilizes high speed machine to shear or the method for chemical oxidation, is separated by the cellulose microfibril in string and disassembles into the elongated fibers of diameter at nanoscale (lower than 100nm).Not only mechanical property is strong for it, draw ratio is high, in aqueous can also in stable colloidal.Utilize the dispersed CNT of suitable method 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 the preparation method providing a kind of biomass nano fiber conductive paper, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A preparation method for biomass nano fiber conductive paper, the distinguishing feature being different from other technique is the layer structure utilizing high speed homogenisation mechanical shearing destroying carbon nanometer tube, makes it present polarity, with cellulose nanometer fibril fiber surface hydroxy combining.Utilize the reunion of the high viscosity retardance CNT of nanofiber mixed solution simultaneously, make its uniform and stable dispersion.Then adopt and be similar to excessive moisture in the method elimination mixed solution of traditional papermaking, obtain the biomass nano fiber conductive paper composite of excellent performance, comprise the following steps:
1st step: dissolved in by thickener hydroxypropyl methylcellulose in cellulose nanometer fibril solution, thickener qualities accounts for the 3-5% of mixed material (dry state).Under high-speed stirred condition, add deionized water above-mentioned mixed solution is diluted to 0.2-0.3wt%.
2nd step: a certain amount of CNT is added in the mixed solution of diluted state cellulose nanometer fibril and thickener, the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
3rd step: high speed homogenisation mechanical shearing process.Mixed solution through preliminary dispersion carries out shearing dispersion treatment in microjet high pressure homogenizer, wherein the reaction chamber conbined usage of 200 μm and 87 μm, circulation shear process 5-8 time.
4th step: through carbon nanotube/nano fibers mixture solution elimination portion of water in pressurization (or vacuum) filtration system of fully dispersion, form colloidal wet film.Wet film under plus load condition through Adsorption of Filter Paper excessive moisture, heat drying to over dry.
In the present invention, in described 1st step, thickener can be hydroxypropyl methylcellulose, hydroxyethylcellulose, carboxy methyl cellulose, or their mixture, but the addition of thickener need control at 3-5wt%, and the viscosity according to raw cellulose nanofibrils solution regulates.
In the present invention, the cellulose nanometer fibril mixed solution after adding thickener in described 1st step need regulate solid content to 0.2-0.3%, blocks in reaction chamber to avoid material in follow-up high speed shear process.
In the present invention, in described 2nd step, the addition of CNT requires depending on target material, and general addition is 3-6wt%, at most can not more than 15wt%.
In the present invention, in described 3rd step during microjet high pressure homogenizer shear treatment, in 200-87 μm of association response chamber, pressure is 140-160MPa.
In the present invention, in described 3rd step during microjet high pressure homogenizer shear treatment, circulation shear number of times is 4-8 time.
In the present invention, in described 4th step, carbon nanotube/nano fibers mixture solution need through cellulose osmosis membrane filters, and wherein the aperture of filter membrane is 0.2-0.7 μm.
In the present invention, in described 4th step, wet film dry run need apply external pressure and prevent its contraction distortion.In order to ensure that in conductive paper, moisture is removed completely, can under 100-105 DEG C 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 homogenisation mechanical shearing destroying carbon nanometer tube, makes it present polarity, can with cellulose nanometer fibril fiber surface hydroxy combining.Simultaneously by the reunion of the high viscosity retardance CNT of nanofiber/cellulose thickener solution, make its uniform and stable dispersion.The cellulose conductive paper production process obtained by this method is simple and easy to control, environmental protection, cost are suitable.Simultaneously, bigger serface, natural cancellated cellulose nanometer fibril can be adsorbed, in conjunction with more CNT, composite conductive 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.
Detailed description of the invention
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
embodiment 1
1st step: dissolved in by thickener hydroxypropyl methylcellulose in cellulose nanometer fibril solution, thickener qualities accounts for 3% of mixed material (dry state).For avoiding material in follow-up high speed shear process to block in reaction chamber, adding deionized water under agitation and above-mentioned mixed solution is diluted to 0.2wt%.
2nd step: the CNT of 5wt% is added in the cellulose nanometer fibril/hydroxypropyl methylcellulose mixed solution of diluted state, the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
3rd step: high speed homogenisation mechanical shearing process.Mixed solution through preliminary dispersion carries out shearing dispersion treatment in microjet high pressure homogenizer, wherein the reaction chamber conbined usage of 200 μm and 87 μm, and reaction pressure is 150MPa, circulation shear process 6 times.
4th step: the carbon nanotube/nano fibers mixture solution through fully disperseing through the cellulosic filter paper elimination portion of water in 0.2 μm of aperture, forms colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under 500N plus load, then under 100-105 DEG C of heating condition further dry 1h.
embodiment 2
1st step: dissolved in by thickener hydroxypropyl methylcellulose in cellulose nanometer fibril solution, thickener qualities accounts for 4% of mixed material (dry state).For avoiding material in follow-up high speed shear process to block in reaction chamber, adding deionized water under agitation and above-mentioned mixed solution is diluted to 0.3wt%.
2nd step: the CNT of 6wt% is added in the cellulose nanometer fibril/hydroxypropyl methylcellulose mixed solution of diluted state, the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
3rd step: high speed homogenisation mechanical shearing process.Mixed solution through preliminary dispersion carries out shearing dispersion treatment in microjet high pressure homogenizer, wherein the reaction chamber conbined usage of 200 μm and 87 μm, and reaction pressure is 150MPa, circulation shear process 8 times.
4th step: the carbon nanotube/nano fibers mixture solution through fully disperseing through the cellulosic filter paper elimination portion of water in 0.4 μm of aperture, forms colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under 500N plus load, then under 100-105 DEG C of heating condition further dry 1h.
embodiment 3
1st step: dissolved in by thickener hydroxypropyl methylcellulose in cellulose nanometer fibril solution, thickener qualities accounts for 5% of mixed material (dry state).For avoiding material in follow-up high speed shear process to block in reaction chamber, adding deionized water under agitation and above-mentioned mixed solution is diluted to 0.2wt%.
2nd step: the CNT of 7wt% is added in the cellulose nanometer fibril/hydroxypropyl methylcellulose mixed solution of diluted state, the preliminary dispersing Nano carbon tubes of mechanical agitation 10min.
3rd step: high speed homogenisation mechanical shearing process.Mixed solution through preliminary dispersion carries out shearing dispersion treatment in microjet high pressure homogenizer, wherein the reaction chamber conbined usage of 200 μm and 87 μm, and reaction pressure is 150MPa, circulation shear process 8 times.
4th step: the carbon nanotube/nano fibers mixture solution through fully disperseing through the cellulosic filter paper elimination portion of water in 0.5 μm of aperture, forms colloidal wet film in Pressure Filter System.Wet film solid content 20%, dry through Adsorption of Filter Paper under 500N plus load, then under 100-105 DEG C of heating condition further dry 1h.
More than show and describe general 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; what describe in above-described embodiment and description 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 application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. a preparation method for biomass nano fiber conductive paper, is characterized in that, comprises the following steps:
1st step: thickener is dissolved in cellulose nanometer fibril solution, thickener qualities accounts for the 3-5% of the mixed material of dry state, under high-speed stirred condition, add deionized water above-mentioned mixed solution is diluted to 0.2-0.3wt%, wherein, thickener is hydroxypropyl methylcellulose, hydroxyethylcellulose, the mixture of carboxy methyl cellulose one of them or they, the viscosity according to raw cellulose nanofibrils solution regulates;
2nd step: a certain amount of CNT is added in the mixed solution of diluted state cellulose nanometer fibril and thickener, the preliminary dispersing Nano carbon tubes of mechanical agitation 10min;
3rd step: high speed homogenisation mechanical shearing process, the mixed solution through preliminary dispersion carries out shearing dispersion treatment in microjet high pressure homogenizer, wherein the reaction chamber conbined usage of 200 μm and 87 μm, circulation shear process 5-8 time;
4th step: through carbon nanotube/nano fibers mixture solution elimination portion of water in pressurization or vacuum filtering system of fully dispersion, form colloidal wet film, wet film under 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, is characterized in that, in described 2nd step, the addition of CNT requires depending on target material, and its addition is less than or equal to 15wt%.
3. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1 and 2, is characterized in that, in described 2nd step, the addition of CNT is 3-6wt%.
4. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described 3rd step during microjet high pressure homogenizer shear treatment, in 200-87 μm of association response chamber, pressure is 140-160MPa.
5. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, is characterized in that, in described 4th step, carbon nanotube/nano fibers mixture solution need through cellulose osmosis membrane filters, and wherein the aperture of filter membrane is 0.2-0.7 μm.
6. the preparation method of a kind of biomass nano fiber conductive paper according to claim 1, it is characterized in that, in described 4th step, wet film dry run need apply external pressure and prevent its contraction distortion, in order to ensure that in conductive paper, moisture is removed completely, can under 100-105 DEG C of heating condition further dry 1h.
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SG11201601418YA (en) * | 2013-10-17 | 2016-03-30 | Univ Nanyang Tech | Conductive paper and method of forming the same |
CN104674582B (en) * | 2013-12-03 | 2017-10-17 | 金东纸业(江苏)股份有限公司 | Paper pulp and preparation method thereof, using paper made from the paper pulp |
CN103966907B (en) * | 2014-04-02 | 2016-08-10 | 上海大学 | A kind of compliant conductive paper based on nano-cellulose and preparation method thereof |
KR101700355B1 (en) | 2014-05-22 | 2017-01-26 | 주식회사 엘지화학 | Preparation method of carbon nanotube and dispersed composition of carbon nanotube |
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 |
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 |
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 |
CN110157393B (en) * | 2019-05-06 | 2021-11-16 | 滨州学院 | Nano fiber-xanthan gum compound viscosity-increasing and cutting-extracting agent for drilling fluid and preparation method thereof |
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 |
CN113881108B (en) * | 2021-10-07 | 2022-07-22 | 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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