CN108976685A - A kind of preparation method of carbon nano-fiber composite material - Google Patents

A kind of preparation method of carbon nano-fiber composite material Download PDF

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CN108976685A
CN108976685A CN201810692769.2A CN201810692769A CN108976685A CN 108976685 A CN108976685 A CN 108976685A CN 201810692769 A CN201810692769 A CN 201810692769A CN 108976685 A CN108976685 A CN 108976685A
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carbon nano
composite material
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刘菊花
张鑫
朱华
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Foshan Teng Carp Amperex Technology Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/02Fibres or whiskers
    • C08K7/04Fibres or whiskers inorganic
    • C08K7/06Elements
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives

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  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The present invention relates to a kind of preparation methods of carbon nano-fiber composite material, belong to technical field of composite materials.The present invention has the characteristic for being easy to form a film with gelation using nano-cellulose, it can be used as the carrier material or skeletal support material of stable structure and good mechanical performance, nano-cellulose has different structural forms, the inorganic or organic nano material of various micro-nano-scales is diffusible or fills wherein, to improve its specific surface area, the original high-hydroscopicity of nano-cellulose, swellability, the characteristics such as biocompatibility, it is mutually fused together with all kinds of inorganic or organic nano material particular conductivity performance, and then it generates with high conductivity, photoelectric conversion, the specific function material of electrochemical redox characteristic, conducting polymer can not only disperse to form conducting membrane material with nano-cellulose by solution, and conducting polymer/nano-cellulose conducing composite material can be obtained by in-situ polymerization mode.

Description

A kind of preparation method of carbon nano-fiber composite material
Technical field
The present invention relates to a kind of preparation methods of carbon nano-fiber composite material, belong to technical field of composite materials.
Background technique
Biomass nano material element is developed from biomass material, and functional product is prepared with this and can further improve biology The added value and utilization efficiency of matter raw material.Biomass resource includes various natural resources and its derives from resource, is distributed on earth Extensively, there is reproducibility, it is inexhaustible.Cellulose is that most wide, the most abundant day of reserves is distributed in nature Right high molecular material is mainly derived from the cell wall of higher plant and timber, if the content of cellulose of cotton is almost up to 100%, For the content of cellulose of timber in 40-50% or so, agricultural waste material (soybean peel, stalk, bagasse) is also the important of cellulose Source.Cellulose in the additive of industrial circle such as weaving, paper and paper pulp, food and pharmaceutical industry there is huge exploitation to answer Use potentiality.
Carbon fiber is to be carbonized by organic fiber or asphaltic base raw material and obtained after graphitization processing, and phosphorus content is high In 85%, it can be used as the reinforcing fiber of composite material.In recent years, researcher passes through the preparation process for improving carbon fiber, in conjunction with elder generation Into analysis means, realize the structure control of carbon fiber.The research trend of carbon fiber just towards high-performance, high function and it is low at The direction of this change is developed.
Nanotechnology is the new and high technology developed since last decade in the world, emerging is had excellent performance as a kind of Material, application prospect is considerable.In the area that the cocos such as Hainan, Guangdong are resourceful, it is falling off naturally, have it is slight The coconut tree branches and leaves of anti-corrosion function are seen everywhere, and seriously affect traffic safety and the city appearance of the city.Related agricultural wastes coconut palm petiole It is seldom that the research of recycling and reusing and high-valued application discloses report.Cellulose is extracted from coconut palm petiole and as preparation Nanowire The raw material for tieing up element, is conducive to changing rejected material to useful resource and Efficient Cycle utilizes, and meets the policy of national sustainable development, has good Environmental benefit.Cellulose is extracted from coconut palm petiole, prepares high intensity, high elastic modulus, the good nano-cellulose of translucency Good, the high-intensitive carbon nano-fiber with electric conductivity, and two kinds of materials progress are compound, and preparation has both high-intensitive and good conductive The nanocomposite of performance can be applied to the fields such as lithium ion battery, supercapacitor.
Summary of the invention
The technical problems to be solved by the invention: mainly added by substances such as coal tar, asphalt for current carbon fiber Work is produced and is obtained, and this kind of resource belongs to non-renewable resources, and a large amount of cocoanut tree waste is incinerated, and causes severe environments The problem of pollution, provides a kind of preparation method of carbon nano-fiber composite material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, 10~20 parts of coconut palm leaves, 40~50 parts of benzene-dehydrated alcohol mixed liquor, 10~15 parts times are weighed respectively Sodium chlorate, 10~15 parts of glacial acetic acid, 6~10 parts of sodium hydroxides, 10~14 parts of hydrochloric acid, by coconut palm leaf and benzene-dehydrated alcohol mixed liquor Sodium hypochlorite and glacial acetic acid are added in the coconut palm leaf extracted, is in temperature for mixing extracting drying and processing, the coconut palm leaf that must have been extracted 1~2h of stir process in 75~85 DEG C of water-baths is washed with deionized to neutrality, and filtering obtains product, by product and hydroxide Sodium mixing, 2~3h of stir process in the water-bath that temperature is 80~90 DEG C are washed with deionized to neutrality, hydrochloric acid are added 2~3h of stir process is washed with deionized to neutrality, obtains cellulose, and grinding, ultrasound and centrifugal treating obtain coconut palm leaf Nanowire Dimension element;
(2) n,N-Dimethylformamide and coconut palm leaf nano-cellulose are mixed, after 40~60min of ultrasonic disperse, carries out Static Spinning Silk preparation, obtains woven fabric;Woven fabric is placed in Muffle furnace, rises to 280~300 DEG C and 2~3h of constant temperature with the heating rate of 1 DEG C/min Afterwards, carbonization-activation is handled, and obtains carbon nano-fiber element;
(3) after mixing by carbon nano-fiber and deionized water, 1~2h of ultrasonic disperse is the adjusting of 37% hydrochloric acid with mass fraction PH is 1~3, obtains dispersion liquid, and polyacrylonitrile is added, and ammonium persulfate is added in 15~30min of magnetic agitation, continue to be stirred to react 3~ 5h is washed 3~5 times, after filtering with acetone and deionized water respectively, be placed in 80~100 DEG C of baking oven dry to constant weight to get Carbon nano-fiber composite material.
The volume ratio of benzene and dehydrated alcohol is 2: 1 in benzene described in step (1)-dehydrated alcohol mixed liquor.
Extracting drying and processing described in step (1) is 5~6h of extracting in 80~90 DEG C of water-bath, and taking-up is placed in 80 It is dried in~100 DEG C of baking ovens.
Grinding described in step (1), ultrasound and centrifugal treating step are grinding 15~20 times, are 1200W ultrasound 1 in power ~2h, and be 10~15min of 8000r/min centrifugal treating in centrifugal speed.
The mass ratio of n,N-Dimethylformamide described in step (2) and coconut palm leaf nano-cellulose is 1: 1.
Electrospinning conditions described in step (2) are negative pressure -3.00~-5.00KV, 23.00~25.00KV of positive pressure, are promoted Rate 0.1mm/min, the distance between syringe needle and receiver are 20~25cm, and temperature is 50~60 DEG C.
The processing of carbonization-activation described in step (2) is to then pass in a nitrogen atmosphere in 600~800 DEG C of 1~2h of charing Carbon dioxide gas activates 2~4h.
Carbon nano-fiber described in step (3) and the mass ratio of deionized water 1: 3.
The mass ratio of polyacrylonitrile described in step (3) and dispersion liquid is 1: 5.
The mass ratio of ammonium persulfate described in step (3) and polyacrylonitrile is 2: 1.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention obtains cellulose from coconut palm leaf using benzene-dehydrated alcohol extracting, soda acid processing, in conjunction with grinding, ultrasound etc. Mechanical treatment extracts nano-cellulose, effectively removes the lignin and hemicellulose in coconut palm leaf, is completely extracted nanometer Cellulose, and reached nano-scale, agricultural wastes coconut palm leaf is taken full advantage of, alleviates environmental problem, is extracted from coconut palm leaf By electrostatic spinning processing, carbonization-activation processing, obtained carbon nano-fiber element has both high-intensitive and well leads nano-cellulose Electrical property;
(2) present invention has using nano-cellulose is easy to film forming and gelation, high-hydroscopicity, swellability, biocompatibility etc. Characteristic, the carrier material or skeletal support material, nano-cellulose that can be used as stable structure and good mechanical performance have The three-dimensional network porous structure of different structural forms, especially diverse microcosmic scale, various micro-nano-scales inorganic or has Machine nano material is diffusible or filling wherein, to improve its specific surface area, the original high-hydroscopicity of nano-cellulose, swellability, The characteristics such as biocompatibility are mutually fused together with all kinds of inorganic or organic nano material particular conductivity performance, and then are produced The raw specific function material with high conductivity, photoelectric conversion, electrochemical redox characteristic, conducting polymer not only can be with Conducting membrane material is formed with nano-cellulose by solution dispersion, and conductive polymer can be obtained by in-situ polymerization mode Son/nano-cellulose conducing composite material.
Specific embodiment
According to parts by weight, 10~20 parts of coconut palm leaves, 40~50 parts of benzene-dehydrated alcohol mixed liquor, 10~15 parts are weighed respectively Coconut palm leaf and volume ratio are 2: 1 benzene-nothing by sodium hypochlorite, 10~15 parts of glacial acetic acid, 6~10 parts of sodium hydroxides, 10~14 parts of hydrochloric acid Water-ethanol mixed liquor extracts 5~6h in 80~90 DEG C of water-bath, and taking-up, which is placed in 80~100 DEG C of baking ovens, dries, and must take out Sodium hypochlorite and glacial acetic acid is added in the coconut palm leaf mentioned in the coconut palm leaf extracted, is to stir in 75~85 DEG C of water-baths in temperature Handle 1~2h, be washed with deionized to neutrality, filtering obtains product, product and sodium hydroxide are mixed, temperature be 80~ 2~3h of stir process in 90 DEG C of water-bath is washed with deionized to neutrality, and 2~3h of hydrochloric acid stir process is added, spend from Sub- water washing obtains cellulose, grinds 20 times, be ultrasound 1h under 1200W in power, and at 8000r/min at centrifugation to neutrality 15min is managed, coconut palm leaf nano-cellulose is obtained;In mass ratio 5: 1 mix n,N-Dimethylformamide and coconut palm leaf nano-cellulose, surpass After sound disperses 40~60min, electrostatic spinning preparation is carried out, woven fabric is obtained;Electrospinning conditions are negative pressure -3.00~-5.00KV, just 23.00~25.00KV is pressed, rate 0.1mm/min is promoted, the distance between syringe needle and receiver are 20~25cm, temperature 50 ~60 DEG C;Woven fabric is placed in Muffle furnace, after rising to 280~300 DEG C and 2~3h of constant temperature with the heating rate of 1 DEG C/min, in nitrogen It in 600~800 DEG C of 1~2h of charing under gas atmosphere, then passes to carbon dioxide gas and activates 2~4h, obtain carbon nano-fiber element;It presses After mixing by carbon nano-fiber and deionized water, 1~2h of ultrasonic disperse is 37% hydrochloric acid tune with mass fraction to mass ratio 1: 3 Save pH be 1~3, obtain dispersion liquid, by the mass ratio of polyacrylonitrile and dispersion liquid be 1: 5 be added polyacrylonitrile, magnetic agitation 15~ 30min, then ammonium persulfates are added for 2: 1 by the mass ratio of ammonium persulfate and polyacrylonitrile, continue to be stirred to react 3~5h, respectively It is washed 3~5 times, after filtering with acetone and deionized water, is placed in 80~100 DEG C of baking oven and dries to constant weight to get carbon nanometer Fibrous composite.
Example 1
According to parts by weight, 10 parts of coconut palm leaves, 40 parts of benzene-dehydrated alcohol mixed liquor, 10 parts of sodium hypochlorite, 10 portions of ice vinegar are weighed respectively Coconut palm leaf and volume ratio are 2: 1 benzene-dehydrated alcohol mixed liquor in 80 DEG C of water-bath by acid, 6 parts of sodium hydroxides, 10 parts of hydrochloric acid Extract 5h, taking-up is placed in 80 DEG C of baking ovens and dries, the coconut palm leaf that must extract, in coconut palm leaf extract addition sodium hypochlorite with Glacial acetic acid is stir process 1h in 75 DEG C of water-baths in temperature, is washed with deionized to neutrality, filtering obtains product, by product It is mixed with sodium hydroxide, the stir process 2h in the water-bath that temperature is 80 DEG C, is washed with deionized to neutrality, hydrochloric acid is added Stir process 2h is washed with deionized to neutrality, obtains cellulose, grinds 20 times, the ultrasound 1h in the case where power is 1200W, and Centrifugal treating 15min under 8000r/min obtains coconut palm leaf nano-cellulose;In mass ratio 5: 1 by n,N-Dimethylformamide and coconut palm leaf Nano-cellulose mixes, and after ultrasonic disperse 40min, carries out electrostatic spinning preparation, obtains woven fabric;Electrospinning conditions are negative pressure- 3.00KV, positive pressure 23.00KV promote rate 0.1mm/min, and the distance between syringe needle and receiver are 20cm, and temperature is 50 DEG C; Woven fabric is placed in Muffle furnace, after rising to 280 DEG C and constant temperature 2h with the heating rate of 1 DEG C/min, in a nitrogen atmosphere in 600 DEG C 1h is carbonized, carbon dioxide gas activation 2h is then passed to, obtains carbon nano-fiber element;In mass ratio 1: 3 carbon nano-fiber and will go After mixing, it is 1 that ultrasonic disperse 1h is 37% salt acid for adjusting pH with mass fraction to ionized water, dispersion liquid is obtained, by polyacrylonitrile Mass ratio with dispersion liquid is 1: 5 addition polyacrylonitrile, magnetic agitation 15min, then the quality by ammonium persulfate and polyacrylonitrile Than ammonium persulfate is added for 2: 1, continues to be stirred to react 3h, washed 3 times, after filtering with acetone and deionized water respectively, be placed in 80 DEG C baking oven in dry to constant weight to get carbon nano-fiber composite material.
Example 2
According to parts by weight, 15 parts of coconut palm leaves, 45 parts of benzene-dehydrated alcohol mixed liquor, 12 parts of sodium hypochlorite, 12 portions of ice vinegar are weighed respectively Coconut palm leaf and volume ratio are 2: 1 benzene-dehydrated alcohol mixed liquor in 85 DEG C of water-bath by acid, 8 parts of sodium hydroxides, 12 parts of hydrochloric acid Extract 5h, taking-up is placed in 90 DEG C of baking ovens and dries, the coconut palm leaf that must extract, in coconut palm leaf extract addition sodium hypochlorite with Glacial acetic acid is stir process 1h in 80 DEG C of water-baths in temperature, is washed with deionized to neutrality, filtering obtains product, by product It is mixed with sodium hydroxide, the stir process 2h in the water-bath that temperature is 85 DEG C, is washed with deionized to neutrality, hydrochloric acid is added Stir process 2h is washed with deionized to neutrality, obtains cellulose, grinds 20 times, the ultrasound 1h in the case where power is 1200W, and Centrifugal treating 15min under 8000r/min obtains coconut palm leaf nano-cellulose;In mass ratio 5: 1 by n,N-Dimethylformamide and coconut palm leaf Nano-cellulose mixes, and after ultrasonic disperse 50min, carries out electrostatic spinning preparation, obtains woven fabric;Electrospinning conditions are negative pressure- 4.00KV, positive pressure 24.00KV promote rate 0.1mm/min, and the distance between syringe needle and receiver are 22cm, and temperature is 55 DEG C; Woven fabric is placed in Muffle furnace, after rising to 290 DEG C and constant temperature 2h with the heating rate of 1 DEG C/min, in a nitrogen atmosphere in 700 DEG C 1h is carbonized, carbon dioxide gas activation 3h is then passed to, obtains carbon nano-fiber element;In mass ratio 1: 3 carbon nano-fiber and will go After mixing, it is 2 that ultrasonic disperse 1h is 37% salt acid for adjusting pH with mass fraction to ionized water, dispersion liquid is obtained, by polyacrylonitrile Mass ratio with dispersion liquid is 1: 5 addition polyacrylonitrile, magnetic agitation 25min, then the quality by ammonium persulfate and polyacrylonitrile Than ammonium persulfate is added for 2: 1, continues to be stirred to react 4h, washed 4 times, after filtering with acetone and deionized water respectively, be placed in 90 DEG C baking oven in dry to constant weight to get carbon nano-fiber composite material.
Example 3
According to parts by weight, 20 parts of coconut palm leaves, 50 parts of benzene-dehydrated alcohol mixed liquor, 15 parts of sodium hypochlorite, 15 portions of ice vinegar are weighed respectively Coconut palm leaf and volume ratio are 2: 1 benzene-dehydrated alcohol mixed liquor in 90 DEG C of water-bath by acid, 10 parts of sodium hydroxides, 14 parts of hydrochloric acid 6h is extracted, taking-up, which is placed in 100 DEG C of baking ovens, dries, and sodium hypochlorite is added in the coconut palm leaf extracted in the coconut palm leaf that must have been extracted And glacial acetic acid, it is stir process 2h in 85 DEG C of water-baths in temperature, is washed with deionized to neutrality, filtering obtains product, will produce Object and sodium hydroxide mixing, the stir process 3h in water-bath at a temperature of 90 °C, are washed with deionized to neutrality, salt are added Sour stir process 3h, is washed with deionized to neutrality, obtains cellulose, grinds 20 times, the ultrasound 1h in the case where power is 1200W, and The centrifugal treating 15min at 8000r/min obtains coconut palm leaf nano-cellulose;In mass ratio 5: 1 by n,N-Dimethylformamide and coconut palm Leaf nano-cellulose mixes, and after ultrasonic disperse 60min, carries out electrostatic spinning preparation, obtains woven fabric;Electrospinning conditions are negative pressure- 5.00KV, positive pressure 25.00KV promote rate 0.1mm/min, and the distance between syringe needle and receiver are 25cm, and temperature is 60 DEG C; Woven fabric is placed in Muffle furnace, after rising to 300 DEG C and constant temperature 3h with the heating rate of 1 DEG C/min, in a nitrogen atmosphere in 800 DEG C 2h is carbonized, carbon dioxide gas activation 4h is then passed to, obtains carbon nano-fiber element;In mass ratio 1: 3 carbon nano-fiber and will go After mixing, it is 3 that ultrasonic disperse 2h is 37% salt acid for adjusting pH with mass fraction to ionized water, dispersion liquid is obtained, by polyacrylonitrile Mass ratio with dispersion liquid is 1: 5 addition polyacrylonitrile, magnetic agitation 30min, then the quality by ammonium persulfate and polyacrylonitrile Than ammonium persulfate is added for 2: 1, continues to be stirred to react 5h, washed 5 times, after filtering with acetone and deionized water respectively, be placed in 100 DEG C baking oven in dry to constant weight to get carbon nano-fiber composite material.
Reference examples: the carbon nano-fiber composite material of Beijing new material company production.
The carbon nano-fiber composite material of example and reference examples is detected, specific detection is as follows:
Tensile property test: stretching batten using omnipotent mechanics machine, and specimen holder guarantees batten between two fixtures Effective length in 25mm or so, use the sensor of 1000N, loading velocity 1mm/min.All samples measurement is at least heavy It is 3 times multiple, calculate the average value of its tensile strength.
Electrical performance testing: using RTS-8 type four-point probe (Chinese four probe scientific & technical corporation) to the conduction of sample Performance is tested, and instrument can calculate the conductivity of composite membrane automatically.
Specific testing result such as table 1.
Table 1
Detection project Example 1 Example 2 Example 3 Reference examples
Tensile strength (MPa) 66.7 65.1 67.8 45.2
Conductivity (s/cm) 175.8 175.6 180.3 110.5
As shown in Table 1, carbon nano-fiber composite material prepared by the present invention has good tensile property and good electric conductivity.

Claims (10)

1. a kind of preparation method of carbon nano-fiber composite material, it is characterised in that specific steps are as follows:
(1) according to parts by weight, 10~20 parts of coconut palm leaves, 40~50 parts of benzene-dehydrated alcohol mixed liquor, 10~15 parts times are weighed respectively Sodium chlorate, 10~15 parts of glacial acetic acid, 6~10 parts of sodium hydroxides, 10~14 parts of hydrochloric acid, by coconut palm leaf and benzene-dehydrated alcohol mixed liquor Sodium hypochlorite and glacial acetic acid are added in the coconut palm leaf extracted, is in temperature for mixing extracting drying and processing, the coconut palm leaf that must have been extracted 1~2h of stir process in 75~85 DEG C of water-baths is washed with deionized to neutrality, and filtering obtains product, by product and hydroxide Sodium mixing, 2~3h of stir process in the water-bath that temperature is 80~90 DEG C are washed with deionized to neutrality, hydrochloric acid are added 2~3h of stir process is washed with deionized to neutrality, obtains cellulose, and grinding, ultrasound and centrifugal treating obtain coconut palm leaf Nanowire Dimension element;
(2) n,N-Dimethylformamide and coconut palm leaf nano-cellulose are mixed, after 40~60min of ultrasonic disperse, carries out Static Spinning Silk preparation, obtains woven fabric;Woven fabric is placed in Muffle furnace, rises to 280~300 DEG C and 2~3h of constant temperature with the heating rate of 1 DEG C/min Afterwards, carbonization-activation is handled, and obtains carbon nano-fiber element;
(3) after mixing by carbon nano-fiber and deionized water, 1~2h of ultrasonic disperse is the adjusting of 37% hydrochloric acid with mass fraction PH is 1~3, obtains dispersion liquid, and polyacrylonitrile is added, and ammonium persulfate is added in 15~30min of magnetic agitation, continue to be stirred to react 3~ 5h is washed 3~5 times, after filtering with acetone and deionized water respectively, be placed in 80~100 DEG C of baking oven dry to constant weight to get Carbon nano-fiber composite material.
2. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (1) The benzene-dehydrated alcohol mixed liquor is the mixed liquor that the volume ratio of benzene and dehydrated alcohol is 2: 1.
3. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (1) The extracting drying and processing is 5~6h of extracting in 80~90 DEG C of water-bath, and taking-up, which is placed in 80~100 DEG C of baking ovens, dries It is dry.
4. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (1) Grinding, ultrasound and the centrifugal treating step is grinding 15~20 times, is 1~2h of 1200W ultrasound in power, and in centrifugation speed Degree is 10~15min of 8000r/min centrifugal treating.
5. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (2) The mass ratio of the n,N-Dimethylformamide and coconut palm leaf nano-cellulose is 1: 1.
6. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (2) The electrospinning conditions are negative pressure -3.00~-5.00KV, 23.00~25.00KV of positive pressure, promote rate 0.1mm/min, The distance between syringe needle and receiver are 20~25cm, and temperature is 50~60 DEG C.
7. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (2) The carbonization-activation processing is that it is living to then pass to carbon dioxide gas in 600~800 DEG C of 1~2h of charing in a nitrogen atmosphere Change 2~4h.
8. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (3) The mass ratio 1: 3 of the carbon nano-fiber and deionized water.
9. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (3) The mass ratio of the polyacrylonitrile and dispersion liquid is 1: 5.
10. a kind of preparation method of carbon nano-fiber composite material according to claim 1, it is characterised in that: step (3) The mass ratio of the ammonium persulfate and polyacrylonitrile is 2: 1.
CN201810692769.2A 2018-06-29 2018-06-29 A kind of preparation method of carbon nano-fiber composite material Pending CN108976685A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114128658A (en) * 2021-11-25 2022-03-04 中国水产科学研究院黑龙江水产研究所 Preparation method of modified coconut shred material for artificial fish nest

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004359939A (en) * 2003-05-15 2004-12-24 Dainichiseika Color & Chem Mfg Co Ltd Biodegradable resin composition and its molded article
CN102787444A (en) * 2012-08-18 2012-11-21 东华大学 Preparation method of porous network structure fiber membrane of nano cellulose/silicon dioxide
CN102978984A (en) * 2012-11-26 2013-03-20 中山大学 Preparation method of surface-modified ball-milling refined plant fibers
CN105869901A (en) * 2016-03-30 2016-08-17 北京化工大学 Carbon nanofiber composite material with controllable structure and preparation method and application therefor
CN107761184A (en) * 2017-10-24 2018-03-06 四川大学 A kind of original liquid coloring composite fibre and preparation method thereof
CN108103616A (en) * 2018-01-12 2018-06-01 北京林业大学 A kind of preparation method of the lignin-base carbon fibre composite of N doping

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004359939A (en) * 2003-05-15 2004-12-24 Dainichiseika Color & Chem Mfg Co Ltd Biodegradable resin composition and its molded article
CN102787444A (en) * 2012-08-18 2012-11-21 东华大学 Preparation method of porous network structure fiber membrane of nano cellulose/silicon dioxide
CN102978984A (en) * 2012-11-26 2013-03-20 中山大学 Preparation method of surface-modified ball-milling refined plant fibers
CN105869901A (en) * 2016-03-30 2016-08-17 北京化工大学 Carbon nanofiber composite material with controllable structure and preparation method and application therefor
CN107761184A (en) * 2017-10-24 2018-03-06 四川大学 A kind of original liquid coloring composite fibre and preparation method thereof
CN108103616A (en) * 2018-01-12 2018-06-01 北京林业大学 A kind of preparation method of the lignin-base carbon fibre composite of N doping

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吴东儒等: ""半纤维素的分离纯化和检测"", 《糖的生物化学》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114128658A (en) * 2021-11-25 2022-03-04 中国水产科学研究院黑龙江水产研究所 Preparation method of modified coconut shred material for artificial fish nest

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Application publication date: 20181211