CN110184849A - A kind of preparation method of conductive paper of carbon fiber - Google Patents
A kind of preparation method of conductive paper of carbon fiber Download PDFInfo
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- CN110184849A CN110184849A CN201910416478.5A CN201910416478A CN110184849A CN 110184849 A CN110184849 A CN 110184849A CN 201910416478 A CN201910416478 A CN 201910416478A CN 110184849 A CN110184849 A CN 110184849A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/46—Non-siliceous fibres, e.g. from metal oxides
- D21H13/50—Carbon fibres
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
Abstract
The invention discloses a kind of preparation methods of conductive paper of carbon fiber, belong to technical field of function materials.The present invention mixes polyene itrile group carbon fiber with sodium hydroxide solution, impregnates, and filters, and washing obtains pretreatment carbon fiber；Carbon fiber will be pre-processed, bacterium solution, glucose solution, water mixed fermentation obtains fermentation mixed liquor；By modified sodium alginate liquid, water soluble phenol resin and aniline are stirred, and obtain adhesive；To ferment mixed liquor, adhesive, modified meerschaum, plants essential oil, emulsifier, isocyanates, phosphatide, and organic acid is stirred, and obtain mixed slurry；Mixed slurry is manufactured paper with pulp molding, it is dry, it carbonizes to get conductive paper of carbon fiber.The conductive paper of carbon fiber of technical solution of the present invention preparation has the characteristics that excellent mechanical property and electric conductivity, has broad prospects in the development of functional material technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of conductive paper of carbon fiber, belong to technical field of function materials.
Background technique
Carbon fiber paper is using carbon fiber or activated carbon fiber and carbon fiber or activated carbon fiber and other plant or non-plant
The functional paper with property of fibres mixture manufacturing.Carbon fiber is deposited in the form of staple fiber is random in carbon fiber paper
It is incomparable using long fibre composite forming material in, isotropism.Carbon fiber is different from plant fiber, its surface
Only contain a small amount of group, cutting action can only be generated in pulping process, wire-dividing broom purification phenomenon cannot be generated, in sheet forming
Hydrogen bond will not be generated between fiber afterwards.Some problems different from plant fiber are faced during carbon fiber is at paper to need to solve
Certainly, two aspects of dispersion and paper strength are concentrated mainly on.Common carbon fiber paper is generally manufactured paper with pulp using wet process, and carbon fiber contains
Amount 5% ~ 60%, carbon fiber it is wet-formed in major problem is that dispersion and forming.It is shaped in actual carbon fiber paper real
Middle discovery is tested, if carbon fiber is too long, is not easy to disperse, be easy agglomerating.If otherwise carbon fiber is too short, is easily dispersed into uniform slurry
Liquid, forming evenness is good, but paper strength is low.
Carbon fiber and its composite material have high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, endurance, creep resistant,
A series of excellent properties such as conductive, heat transfer and thermal expansion coefficient are small.Carbon fiber (the density 2.702g/cm of aluminium lighter than aluminium3, steel
Density 7.8g/cm3, 1.76~1.96g/cm of density of carbon fiber3), stronger than steel (tension elastomeric limit σ R=1GPa of stainless steel,
Elastic modulus E=200GPa；Tension elastomeric limit σ R=7GPa of carbon fiber, elastic modulus E=700GPa), it is thinner than the hair of people
(20~50 μm of human hair diameter, 7~8 μm of carbon fiber diameter).In addition there are following features for carbon fiber: high temperature resistant, can make at 2000 DEG C
With not molten not soft in 3000 DEG C of nonoxidizing atmospheres；It is acidproof, it is resistant to the erosion of concentrated hydrochloric acid, sulfuric acid, phosphoric acid solution；Thermal expansion system
Number is small, is approximately equal to zero；Thermal conductivity is high, and coefficient of friction is small, good conductivity.Since carbon fiber not only has the intrinsic spy of carbon materials
Property, and electric conductivity and thermal conductivity with metal material, so, all using carbon fiber as being both Developing Space, aviation and military affairs
The essential new material of sophisticated technology is also considered as the basic material of civilian industry update.
Carbon fiber paper can be widely used for antistatic packaging, electromagnetic shielding, planar heating, heat-proof combustion-resistant, new energy, electrification
The materials such as, biomedicine.Carbon fiber has an a variety of advantageous excellent performances, therefore carbon fiber paper and its composite material are ground
Study carefully and using extensive attention has been caused, has developed antistatic packaging material and shielding material, novel laminated planar hair
In hot material, fuel cell as the gas diffusion layers carbon fiber paper of proton exchange membrane, heat-resisting and fire-retardant composite, for Water warfare and
The activated carbon fiber filter paper (ACF) of air cleaning, high-fidelity loudspeaker material etc..
And conventional conductive carbon fiber paper mechanical property and electric conductivity the problem of can not further increasing.Therefore, how to change
The shortcomings that kind conventional conductive carbon fiber paper is that it is promoted and is applied to broader neck to obtain the promotion of more high combination property
Domain meets industrial production demand urgent problem to be solved.
Summary of the invention
The present invention solves the technical problem of: it can not for conventional conductive carbon fiber paper mechanical property and electric conductivity
The problem of further increasing provides a kind of preparation method of conductive paper of carbon fiber.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of conductive paper of carbon fiber, specific preparation process is as follows:
(1) polyene itrile group carbon fiber is mixed with sodium hydroxide solution 1:10~1:20 in mass ratio, is impregnated, filtered, washing obtains
Pre-process carbon fiber；
(2) according to parts by weight, by 20~30 parts of pretreatment carbon fibers, 4~5 parts of bacterium solutions, 3~5 parts of glucose solutions, 20~30
Part water mixed fermentation, obtains fermentation mixed liquor；
(3) according to parts by weight, by 10~20 parts of modified sodium alginate liquid, 30~40 parts of water soluble phenol resins and 5~8 parts of benzene
Amine is stirred, and obtains adhesive；
(4) according to parts by weight, by 20~30 portions of fermentation mixed liquors, 10~20 parts of adhesives, 3~5 parts of modified meerschaums, 2~3
Part plants essential oil, 2~3 parts of emulsifiers, 2~3 parts of isocyanates, 2~3 parts of phosphatide, 2~3 parts of organic acids are stirred, obtain mixed
Close slurry；
(5) mixed slurry is manufactured paper with pulp molding, it is dry, it carbonizes to get conductive paper of carbon fiber.
Step (2) described bacterium solution is made of the raw material of following parts by weight: 1~2 part of bacillus subtilis, 2~3 parts sweet
Oil, 1~2 part of polyethylene glycol, 10~20 parts of deionized waters.
The preparation process of step (3) the modified sodium alginate liquid are as follows: by sodium alginate and water 1:50~1 in mass ratio:
100 mixing, after standing swelling, heating stirring dissolution is subsequently added into 0.1~0.2 times of sodium alginate quality of sodium metaperiodate, heats
It is stirred to react to get modified sodium alginate liquid.
The preparation process of step (4) described modified meerschaum are as follows: by sepiolite and nano ferriferrous oxide in mass ratio 10:
1~20:1 is crushed, and is sieved, and roasting obtains pretreatment sepiolite, according to parts by weight, by 30~40 parts of pretreatment sepiolites, 10~
Salt acid for adjusting pH is then added dropwise to 3.8 in 20 parts of silane resin acceptor kh-550s, 20~30 parts of dehydrated alcohols, 40~60 parts of water mixing
~4.0, constant temperature is stirred to react, and is filtered, washing, dry to get modified meerschaum.
Step (4) plants essential oil is Rosemary Oil, Lavender, rose ethereal oil, jasmine essential oil, camellia
Any one in essential oil or saussurea involucrata essential oil.
Step (4) emulsifier is emulsifier op-10, any one in Tween-80 or Tween-60.
Step (4) described carbonization condition are as follows: temperature is 1000~1100 DEG C, and the time is 2~3h.
Step (4) isocyanates is toluene di-isocyanate(TDI), methyl diphenylene diisocyanate or trimethyl cyclohexane
Any one in diisocyanate.
Step (4) phosphatide is milk phosphatide, any one in peanut phosphatide or yolk phospholipid.
Step (4) organic acid is citric acid, ethylenediamine tetra-acetic acid, poly or polyacrylic acid, hydroxy ethylene
Any one in diphosphonic acid.
The beneficial effects of the present invention are:
(1) present invention is by addition bacterium solution, during the preparation process, firstly, carbon fiber, bacterium solution, glucose solution, water will be pre-processed
Mixed fermentation enables the bacillus subtilis in bacterium solution to breed inside pretreatment of fiber, secondly, in use,
Under the conditions of certain temperature, laccase is generated in the bacillus subtilis metabolic process in mixed bacteria liquid, aniline can be shifted to laccase
Electronics forms aniline free radical, and aniline free radical can cause aniline polymerization, extends outward to form three inside pretreatment carbon fiber
Tie up network, on the one hand, so that generate polyaniline and pretreatment carbon fiber interface cohesion it is even closer, reduce polyaniline in advance
Interface resistance between Treatment of Carbon, so that the electric conductivity of system is further promoted, on the other hand, polyaniline
Three-dimensional network can be formed with modified sodium alginate, the water soluble phenol resin in system and intersect entanglement, so that the friendship in system
Networking network further densifies, so that the mechanical property of system gets a promotion；
(2) present invention is during the preparation process first mixed nano ferriferrous oxide with sepiolite by adding modified meerschaum
Ball-milling treatment enables ferroso-ferric oxide to disperse in sepiolite system, and sepiolite disperses to form sepiolite fibre beam in water,
Meanwhile sepiolite inherently has good rheological characteristic and highly viscous suspension stability, improves its hydrophilic surface by coupling agent
Afterwards, the suspension system of stable dispersion can be formed in resin system, and carrying is nano ferriferrous oxide suspended dispersed, in matrix
After solidification, the sepiolite fibre Shu Zuhe for carrying nano ferriferrous oxide forms sepiolite fibre beam conduction, so that system
Electric conductivity further promoted；
(3) present invention is by addition modified sodium alginate liquid and plants essential oil, and in use, plant-derived essential oil occupies
The position of amount of activated group in modified sodium alginate skeleton, the vibration for reducing covalent bond in modified sodium alginate molecule are strong
Degree, meanwhile, the free H group that can form hydrophilic bond with water can be made to reduce in modified sodium alginate, at the same make film contact angle and
Swelling index reduces, so that the water content of system reduces, so that the mechanical property of system is further promoted.
Specific embodiment
Sodium alginate and water 1:50~1:100 in mass ratio are placed in No. 1 beaker, stir 10~20min with glass bar,
After standing 3~5h of swelling, No. 1 beaker is placed in digital display and is tested the speed in constant temperature blender with magnetic force, is 90~95 DEG C in temperature, revolving speed is
Under the conditions of 400~600r/min, heating stirring dissolves 40~60min, and sodium alginate quality 0.1 will then be added in No. 1 beaker
~0.2 times of sodium metaperiodate, in temperature be 90~95 DEG C, revolving speed be 400~600r/min under the conditions of, heating stirring reaction 40~
60min is placed in ball mill to get modified sodium alginate liquid, by sepiolite and nano ferriferrous oxide 10:1~20:1 in mass ratio
Middle ball mill grinding, cross 120 mesh sieve, obtain refinement sepiolite, then will refinement sepiolite be placed in Muffle furnace, in temperature be 650
Under the conditions of~750 DEG C, 2~3h is roasted, pretreatment sepiolite is obtained, according to parts by weight, by 30~40 parts of pretreatment sepiolites, 10
~20 parts of silane resin acceptor kh-550s, 20~30 parts of dehydrated alcohols, 40~60 parts of water are placed in No. 2 beakers, in revolving speed be 300~
Under the conditions of 500r/min, it is stirred 40~60min, the hydrochloric acid tune that mass fraction is 10~20% is then added dropwise into No. 2 beakers
PH to 3.8~4.0 is saved, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, is 60~80 DEG C in temperature, turns
Under the conditions of speed is 400~600r/min, constant temperature is stirred to react 1~2h, obtains mixed serum, then mixed serum is filtered, obtains filter cake,
Then by filter cake be washed with deionized 3~5 times washing, then the filter cake after washing is placed in baking oven, in temperature be 105~
Under the conditions of 110 DEG C, drying is to constant weight to get modified meerschaum；In mass ratio by polyene itrile group carbon fiber and sodium hydroxide solution
1:10~1:20 is placed in reaction kettle, under the conditions of revolving speed is 400~600r/min, after being stirred 2~3h of immersion, and filtering,
Filter residue is obtained, is then neutrality by residue washing to cleaning solution with glacial acetic acid, obtains pretreatment carbon fiber；According to parts by weight, by 20
~30 parts of pretreatment carbon fibers, 4~5 parts of bacterium solutions, 3~5 parts of glucose solutions, 20~30 parts of water are placed in fermentation cauldron, Yu Wendu
It is 30~35 DEG C, under the conditions of revolving speed is 200~300r/min, mixed fermentation 3~5 days, obtains fermentation mixed liquor；In parts by weight
Meter, by 10~20 parts of modified sodium alginate liquid, 30~40 parts of water soluble phenol resins and 5~8 parts of aniline are placed in No. 3 beakers,
Under the conditions of revolving speed is 600~800r/min, it is stirred 40~60min, obtains adhesive；According to parts by weight, by 20~30
Part fermentation mixed liquor, 10~20 parts of adhesives, 3~5 parts of modified meerschaums, 2~3 parts of plants essential oils, 2~3 parts of emulsifiers, 2~3
Part isocyanates, 2~3 parts of phosphatide, 2~3 parts of organic acids are placed in batch mixer, under the conditions of revolving speed is 400~600r/min, are stirred
40~60min of mixing is mixed, mixed slurry is obtained；Mixed slurry is manufactured paper with pulp molding, blank is obtained, then blank is placed in baking oven, in
Under the conditions of temperature is 60~80 DEG C, the blank after drying is then placed in retort by dry 40~60min, and with 60~
The rate of 90mL/min is filled with nitrogen into furnace, and is warming up to 1000~1100 DEG C with the rate of 8~10 DEG C/min, is in temperature
Under the conditions of 1000~1100 DEG C, after carbonizing 2~3h, room temperature is down to get conductive paper of carbon fiber with furnace.The bacterium solution is by following
The raw materials of parts by weight forms: 1~2 part of bacillus subtilis, 2~3 parts of glycerol, 1~2 part of polyethylene glycol, 10~20 parts go from
Sub- water.The plants essential oil is Rosemary Oil, Lavender, rose ethereal oil, jasmine essential oil, camellia essential oil or saussurea involucrata
Any one in essential oil.The emulsifier is emulsifier op-10, any one in Tween-80 or Tween-60.The isocyanide
Acid esters is toluene di-isocyanate(TDI), any one in methyl diphenylene diisocyanate or trimethylhexane diisocyanate.
The phosphatide is milk phosphatide, any one in peanut phosphatide or yolk phospholipid.The organic acid is citric acid, ethylenediamine tetraacetic
Acetic acid, poly or polyacrylic acid, any one in hydroxy ethylidene-diphosphate.
Example 1
Sodium alginate and water 1:100 in mass ratio are placed in No. 1 beaker, stir 20min with glass bar, after standing swelling 5h,
No. 1 beaker is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 95 DEG C, under the conditions of revolving speed is 600r/min, heating
Then 0.2 times of sodium alginate quality of sodium metaperiodate will be added in stirring and dissolving 60min in No. 1 beaker, be 95 DEG C in temperature, turn
Under the conditions of speed is 600r/min, heating stirring reacts 60min to get modified sodium alginate liquid, and sepiolite and nanometer four are aoxidized
Three-iron 20:1 in mass ratio is placed in ball mill grinding in ball mill, crosses the sieve of 120 mesh, obtains refinement sepiolite, will then refine Hai Pao
Stone is placed in Muffle furnace, under the conditions of temperature is 750 DEG C, is roasted 3h, pretreatment sepiolite is obtained, according to parts by weight, by 40 parts
Pretreatment sepiolite, 20 parts of silane resin acceptor kh-550s, 30 parts of dehydrated alcohols, 60 parts of water are placed in No. 2 beakers, are in revolving speed
Under the conditions of 500r/min, it is stirred 60min, the salt acid for adjusting pH that then dropwise addition mass fraction is 20% into No. 2 beakers is extremely
4.0, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, are 80 DEG C in temperature, revolving speed is 600r/min condition
Under, constant temperature is stirred to react 2h, obtains mixed serum, then mixed serum is filtered, obtains filter cake, then filter cake is washed with deionized
Filter cake after washing, is then placed in baking oven by 5 washings, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modification
Sepiolite；Polyene itrile group carbon fiber and sodium hydroxide solution 1:20 in mass ratio are placed in reaction kettle, in revolving speed be 600r/
Under the conditions of min, it is stirred after impregnating 3h, it is then neutrality by residue washing to cleaning solution with glacial acetic acid that filtering, which obtains filter residue,
Carbon fiber must be pre-processed；According to parts by weight, by 30 parts of pretreatment carbon fibers, 5 parts of bacterium solutions, 5 parts of glucose solutions, 30 parts of water are set
In fermentation cauldron, it is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, mixed fermentation 5 days, obtains fermentation mixed liquor；By weight
Number meter, by 20 parts of modified sodium alginate liquid, 40 parts of water soluble phenol resins and 8 parts of aniline are placed in No. 3 beakers, are in revolving speed
Under the conditions of 800r/min, it is stirred 60min, obtains adhesive；According to parts by weight, by 30 portions of fermentation mixed liquors, 20 parts of bondings
Agent, 5 parts of modified meerschaums, 3 parts of plants essential oils, 3 parts of emulsifiers, 3 parts of isocyanates, 3 parts of phosphatide, 3 parts of organic acids are placed in mixing
In machine, under the conditions of revolving speed is 600r/min, it is stirred 60min, obtains mixed slurry；Mixed slurry is manufactured paper with pulp molding, base is obtained
Blank, is then placed in baking oven by material, and under the conditions of temperature is 80 DEG C, the blank after drying is then placed in charcoal by dry 60min
Change in furnace, and nitrogen is filled with into furnace with the rate of 90mL/min, and be warming up to 1100 DEG C with the rate of 10 DEG C/min, Yu Wendu
Under the conditions of 1100 DEG C, after carbonizing 3h, room temperature is down to get conductive paper of carbon fiber with furnace.The bacterium solution is by following parts by weight
Several raw material composition: 2 parts of bacillus subtilises, 3 parts of glycerol, 2 parts of polyethylene glycol, 20 parts of deionized waters.The plants essential oil is
Rosemary Oil.The emulsifier is emulsifier op-10.The isocyanates is toluene di-isocyanate(TDI).The phosphatide is ox
Milk phosphatide.The organic acid is citric acid.
Example 2
Sodium alginate and water 1:100 in mass ratio are placed in No. 1 beaker, stir 20min with glass bar, after standing swelling 5h,
No. 1 beaker is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 95 DEG C, under the conditions of revolving speed is 600r/min, heating
Then 0.2 times of sodium alginate quality of sodium metaperiodate will be added in stirring and dissolving 60min in No. 1 beaker, be 95 DEG C in temperature, turn
Under the conditions of speed is 600r/min, heating stirring reacts 60min to get modified sodium alginate liquid, and sepiolite and nanometer four are aoxidized
Three-iron 20:1 in mass ratio is placed in ball mill grinding in ball mill, crosses the sieve of 120 mesh, obtains refinement sepiolite, will then refine Hai Pao
Stone is placed in Muffle furnace, under the conditions of temperature is 750 DEG C, is roasted 3h, pretreatment sepiolite is obtained, according to parts by weight, by 40 parts
Pretreatment sepiolite, 20 parts of silane resin acceptor kh-550s, 30 parts of dehydrated alcohols, 60 parts of water are placed in No. 2 beakers, are in revolving speed
Under the conditions of 500r/min, it is stirred 60min, the salt acid for adjusting pH that then dropwise addition mass fraction is 20% into No. 2 beakers is extremely
4.0, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, are 80 DEG C in temperature, revolving speed is 600r/min condition
Under, constant temperature is stirred to react 2h, obtains mixed serum, then mixed serum is filtered, obtains filter cake, then filter cake is washed with deionized
Filter cake after washing, is then placed in baking oven by 5 washings, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modification
Sepiolite；Polyene itrile group carbon fiber and sodium hydroxide solution 1:20 in mass ratio are placed in reaction kettle, in revolving speed be 600r/
Under the conditions of min, it is stirred after impregnating 3h, it is then neutrality by residue washing to cleaning solution with glacial acetic acid that filtering, which obtains filter residue,
Carbon fiber must be pre-processed；According to parts by weight, by 30 parts of pretreatment carbon fibers, 5 parts of glucose solutions, 30 parts of water are placed in fermentation cauldron
In, it is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, mixed fermentation 5 days, obtains fermentation mixed liquor；According to parts by weight, will
20 parts of modified sodium alginate liquid, 40 parts of water soluble phenol resins and 8 parts of aniline are placed in No. 3 beakers, in revolving speed be 800r/min
Under the conditions of, it is stirred 60min, obtains adhesive；According to parts by weight, by 30 portions of fermentation mixed liquors, 20 parts of adhesives, 5 parts change
Property sepiolite, 3 parts of plants essential oils, 3 parts of emulsifiers, 3 parts of isocyanates, 3 parts of phosphatide, 3 parts of organic acids are placed in batch mixer, in turning
Under the conditions of speed is 600r/min, it is stirred 60min, obtains mixed slurry；Mixed slurry is manufactured paper with pulp molding, blank is obtained, then will
Blank is placed in baking oven, and under the conditions of temperature is 80 DEG C, the blank after drying is then placed in retort by dry 60min, and
Be filled with nitrogen into furnace with the rate of 90mL/min, and be warming up to 1100 DEG C with the rate of 10 DEG C/min, in temperature be 1100 DEG C
Under the conditions of, after carbonizing 3h, room temperature is down to get conductive paper of carbon fiber with furnace.The plants essential oil is Rosemary Oil.The cream
Agent is emulsifier op-10.The isocyanates is toluene di-isocyanate(TDI).The phosphatide is milk phosphatide.The organic acid
For citric acid.
Example 3
Sepiolite and nano ferriferrous oxide 20:1 in mass ratio are placed in ball mill grinding in ball mill, the sieve of 120 mesh is crossed, obtains carefully
Change sepiolite, then refinement sepiolite is placed in Muffle furnace, under the conditions of temperature is 750 DEG C, roasts 3h, Hai Pao must be pre-processed
Stone, according to parts by weight, by 40 parts of pretreatment sepiolites, 20 parts of silane resin acceptor kh-550s, 30 parts of dehydrated alcohols, 60 parts of water are set
In No. 2 beakers, under the conditions of revolving speed is 500r/min, it is stirred 60min, mass fraction then is added dropwise into No. 2 beakers
For 20% salt acid for adjusting pH to 4.0, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, in temperature be 80
DEG C, under the conditions of revolving speed is 600r/min, constant temperature is stirred to react 2h, obtains mixed serum, then mixed serum is filtered, obtains filter cake, connect
By filter cake be washed with deionized 5 times washing, then the filter cake after washing is placed in baking oven, in temperature be 110 DEG C of conditions
Under, drying is to constant weight to get modified meerschaum；Polyene itrile group carbon fiber and sodium hydroxide solution 1:20 in mass ratio are placed in instead
It answers in kettle, under the conditions of revolving speed is 600r/min, is stirred after impregnating 3h, filtering obtains filter residue, then with glacial acetic acid by filter residue
Washing to cleaning solution is neutrality, obtains pretreatment carbon fiber；According to parts by weight, by 30 parts of pretreatment carbon fibers, 5 parts of bacterium solutions, 5 parts
Glucose solution, 30 parts of water are placed in fermentation cauldron, in temperature be 35 DEG C, revolving speed be 300r/min under the conditions of, mixed fermentation 5 days,
Must ferment mixed liquor；According to parts by weight, 40 parts of water soluble phenol resins and 8 parts of aniline are placed in No. 3 beakers, are in revolving speed
Under the conditions of 800r/min, it is stirred 60min, obtains adhesive；According to parts by weight, by 30 portions of fermentation mixed liquors, 20 parts of bondings
Agent, 5 parts of modified meerschaums, 3 parts of plants essential oils, 3 parts of emulsifiers, 3 parts of isocyanates, 3 parts of phosphatide, 3 parts of organic acids are placed in mixing
In machine, under the conditions of revolving speed is 600r/min, it is stirred 60min, obtains mixed slurry；Mixed slurry is manufactured paper with pulp molding, base is obtained
Blank, is then placed in baking oven by material, and under the conditions of temperature is 80 DEG C, the blank after drying is then placed in charcoal by dry 60min
Change in furnace, and nitrogen is filled with into furnace with the rate of 90mL/min, and be warming up to 1100 DEG C with the rate of 10 DEG C/min, Yu Wendu
Under the conditions of 1100 DEG C, after carbonizing 3h, room temperature is down to get conductive paper of carbon fiber with furnace.The bacterium solution is by following parts by weight
Several raw material composition: 2 parts of bacillus subtilises, 3 parts of glycerol, 2 parts of polyethylene glycol, 20 parts of deionized waters.The plants essential oil is
Rosemary Oil.The emulsifier is emulsifier op-10.The isocyanates is toluene di-isocyanate(TDI).The phosphatide is ox
Milk phosphatide.The organic acid is citric acid.
Example 4
Sodium alginate and water 1:100 in mass ratio are placed in No. 1 beaker, stir 20min with glass bar, after standing swelling 5h,
No. 1 beaker is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 95 DEG C, under the conditions of revolving speed is 600r/min, heating
Then 0.2 times of sodium alginate quality of sodium metaperiodate will be added in stirring and dissolving 60min in No. 1 beaker, be 95 DEG C in temperature, turn
Under the conditions of speed is 600r/min, heating stirring reacts 60min to get modified sodium alginate liquid, by polyene itrile group carbon fiber and hydrogen
Sodium hydroxide solution 1:20 in mass ratio is placed in reaction kettle, under the conditions of revolving speed is 600r/min, is stirred after impregnating 3h, mistake
Filter, obtains filter residue, is then neutrality by residue washing to cleaning solution with glacial acetic acid, obtains pretreatment carbon fiber；According to parts by weight, will
30 parts of pretreatment carbon fibers, 5 parts of bacterium solutions, 5 parts of glucose solutions, 30 parts of water are placed in fermentation cauldron, are 35 DEG C in temperature, revolving speed is
Under the conditions of 300r/min, mixed fermentation 5 days, fermentation mixed liquor is obtained；According to parts by weight, by 20 parts of modified sodium alginate liquid, 40
Part water soluble phenol resin and 8 parts of aniline are placed in No. 3 beakers, under the conditions of revolving speed is 800r/min, are stirred 60min,
Obtain adhesive；According to parts by weight, by 30 portions of fermentation mixed liquors, 20 parts of adhesives, 3 parts of plants essential oils, 3 parts of emulsifiers, 3 parts different
Cyanate, 3 parts of phosphatide, 3 parts of organic acids are placed in batch mixer, under the conditions of revolving speed is 600r/min, is stirred 60min, is obtained
Mixed slurry；Mixed slurry is manufactured paper with pulp molding, blank is obtained, then blank is placed in baking oven, under the conditions of temperature is 80 DEG C, is done
Blank after drying is then placed in retort by dry 60min, and is filled with nitrogen into furnace with the rate of 90mL/min, and with
The rate of 10 DEG C/min is warming up to 1100 DEG C, under the conditions of temperature is 1100 DEG C, after carbonizing 3h, is down to room temperature with furnace to get leading
Electric carbon fiber paper.The bacterium solution is made of the raw material of following parts by weight: 2 parts of bacillus subtilises, 3 parts of glycerol, 2 parts of poly- second
Glycol, 20 parts of deionized waters.The plants essential oil is Rosemary Oil.The emulsifier is emulsifier op-10.The isocyanic acid
Ester is toluene di-isocyanate(TDI).The phosphatide is milk phosphatide.The organic acid is citric acid.
Example 5
Sodium alginate and water 1:100 in mass ratio are placed in No. 1 beaker, stir 20min with glass bar, after standing swelling 5h,
No. 1 beaker is placed in digital display to test the speed in constant temperature blender with magnetic force, in temperature be 95 DEG C, under the conditions of revolving speed is 600r/min, heating
Then 0.2 times of sodium alginate quality of sodium metaperiodate will be added in stirring and dissolving 60min in No. 1 beaker, be 95 DEG C in temperature, turn
Under the conditions of speed is 600r/min, heating stirring reacts 60min to get modified sodium alginate liquid, and sepiolite and nanometer four are aoxidized
Three-iron 20:1 in mass ratio is placed in ball mill grinding in ball mill, crosses the sieve of 120 mesh, obtains refinement sepiolite, will then refine Hai Pao
Stone is placed in Muffle furnace, under the conditions of temperature is 750 DEG C, is roasted 3h, pretreatment sepiolite is obtained, according to parts by weight, by 40 parts
Pretreatment sepiolite, 20 parts of silane resin acceptor kh-550s, 30 parts of dehydrated alcohols, 60 parts of water are placed in No. 2 beakers, are in revolving speed
Under the conditions of 500r/min, it is stirred 60min, the salt acid for adjusting pH that then dropwise addition mass fraction is 20% into No. 2 beakers is extremely
4.0, No. 2 beakers are then placed in digital display and are tested the speed in constant temperature blender with magnetic force, are 80 DEG C in temperature, revolving speed is 600r/min condition
Under, constant temperature is stirred to react 2h, obtains mixed serum, then mixed serum is filtered, obtains filter cake, then filter cake is washed with deionized
Filter cake after washing, is then placed in baking oven by 5 washings, and under the conditions of temperature is 110 DEG C, drying is to constant weight to get modification
Sepiolite；Polyene itrile group carbon fiber and sodium hydroxide solution 1:20 in mass ratio are placed in reaction kettle, in revolving speed be 600r/
Under the conditions of min, it is stirred after impregnating 3h, it is then neutrality by residue washing to cleaning solution with glacial acetic acid that filtering, which obtains filter residue,
Carbon fiber must be pre-processed；According to parts by weight, by 30 parts of pretreatment carbon fibers, 5 parts of bacterium solutions, 5 parts of glucose solutions, 30 parts of water are set
In fermentation cauldron, it is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, mixed fermentation 5 days, obtains fermentation mixed liquor；By weight
Number meter, by 20 parts of modified sodium alginate liquid, 40 parts of water soluble phenol resins and 8 parts of aniline are placed in No. 3 beakers, are in revolving speed
Under the conditions of 800r/min, it is stirred 60min, obtains adhesive；According to parts by weight, by 30 portions of fermentation mixed liquors, 20 parts of bondings
Agent, 5 parts of modified meerschaums, 3 parts of emulsifiers, 3 parts of isocyanates, 3 parts of phosphatide, 3 parts of organic acids are placed in batch mixer, are in revolving speed
Under the conditions of 600r/min, it is stirred 60min, obtains mixed slurry；Mixed slurry is manufactured paper with pulp molding, blank is obtained, then by blank
It is placed in baking oven, under the conditions of temperature is 80 DEG C, the blank after drying is then placed in retort by dry 60min, and with
The rate of 90mL/min is filled with nitrogen into furnace, and is warming up to 1100 DEG C with the rate of 10 DEG C/min, in temperature be 1100 DEG C of items
Under part, after carbonizing 3h, room temperature is down to get conductive paper of carbon fiber with furnace.The bacterium solution is the raw material group by following parts by weight
At: 2 parts of bacillus subtilises, 3 parts of glycerol, 2 parts of polyethylene glycol, 20 parts of deionized waters.The emulsifier is emulsifier op-10.
Comparative example: the conductive paper of carbon fiber of Wenzhou material production Co., Ltd production.The isocyanates is toluene two
Isocyanates.The phosphatide is milk phosphatide.The organic acid is citric acid.
Example 1 to the resulting conductive paper of carbon fiber of example 5 and comparative example product are subjected to performance detection, specific detection method
It is as follows:
Tensile index according to GB/T22898 detection test specimen;With the sheet resistance of four probe method detection test specimen.
Specific testing result is as shown in table 1:
The specific testing result of 1 conductive paper of carbon fiber of table
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Tensile strength/Nm/g | 17.8 | 13.5 | 15.7 | 12.4 | 13.8 | 7.5 |
| Resistivity/Ω cm | 23.4 | 56.7 | 38.9 | 156.3 | 104.7 | 184.6 |
By 1 testing result of table it is found that the conductive paper of carbon fiber of technical solution of the present invention preparation has excellent mechanical property and leads
The characteristics of electrical property, has broad prospects in the development of functional material technology industry.
Claims (10)
1. a kind of preparation method of conductive paper of carbon fiber, it is characterised in that specific preparation process is as follows:
(1) polyene itrile group carbon fiber is mixed with sodium hydroxide solution 1:10~1:20 in mass ratio, is impregnated, filtered, washing obtains
Pre-process carbon fiber；
(2) according to parts by weight, by 20~30 parts of pretreatment carbon fibers, 4~5 parts of bacterium solutions, 3~5 parts of glucose solutions, 20~30
Part water mixed fermentation, obtains fermentation mixed liquor；
(3) according to parts by weight, by 10~20 parts of modified sodium alginate liquid, 30~40 parts of water soluble phenol resins and 5~8 parts of benzene
Amine is stirred, and obtains adhesive；
(4) according to parts by weight, by 20~30 portions of fermentation mixed liquors, 10~20 parts of adhesives, 3~5 parts of modified meerschaums, 2~3
Part plants essential oil, 2~3 parts of emulsifiers, 2~3 parts of isocyanates, 2~3 parts of phosphatide, 2~3 parts of organic acids are stirred, obtain mixed
Close slurry；
(5) mixed slurry is manufactured paper with pulp molding, it is dry, it carbonizes to get conductive paper of carbon fiber.
2. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (2) described bacterium solution
It is made of the raw material of following parts by weight: 1~2 part of bacillus subtilis, 2~3 parts of glycerol, 1~2 part of polyethylene glycol, 10~
20 parts of deionized waters.
3. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (3) described modification
The preparation process of sodium alginate solution are as follows: sodium alginate is mixed with water 1:50~1:100 in mass ratio, after standing swelling, heating
Stirring and dissolving is subsequently added into 0.1~0.2 times of sodium alginate quality of sodium metaperiodate, and heating stirring reaction is to get modified alginic acid
Sodium liquid.
4. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described modification
The preparation process of sepiolite are as follows: sepiolite and nano ferriferrous oxide 10:1~20:1 in mass ratio are crushed, are sieved, roasting,
Sepiolite must be pre-processed, according to parts by weight, by 30~40 parts of pretreatment sepiolites, 10~20 parts of silane resin acceptor kh-550s,
Salt acid for adjusting pH is then added dropwise to 3.8~4.0 in 20~30 parts of dehydrated alcohols, 40~60 parts of water mixing, and constant temperature is stirred to react, mistake
Filter, washing are dry to get modified meerschaum.
5. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described plant
Essential oil is Rosemary Oil, Lavender, rose ethereal oil, jasmine essential oil, any in camellia essential oil or saussurea involucrata essential oil
It is a kind of.
6. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described emulsification
Agent is emulsifier op-10, any one in Tween-80 or Tween-60.
7. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described charing
Condition are as follows: temperature is 1000~1100 DEG C, and the time is 2~3h.
8. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described isocyanide
Acid esters is toluene di-isocyanate(TDI), any one in methyl diphenylene diisocyanate or trimethylhexane diisocyanate.
9. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) described phosphatide
Any one for milk phosphatide, in peanut phosphatide or yolk phospholipid.
10. a kind of preparation method of conductive paper of carbon fiber according to claim 1, it is characterised in that: step (4) is described organic
Acid is citric acid, ethylenediamine tetra-acetic acid, poly or polyacrylic acid, any one in hydroxy ethylidene-diphosphate.
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