CN106192212B - A kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode - Google Patents
A kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode Download PDFInfo
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- CN106192212B CN106192212B CN201610542494.5A CN201610542494A CN106192212B CN 106192212 B CN106192212 B CN 106192212B CN 201610542494 A CN201610542494 A CN 201610542494A CN 106192212 B CN106192212 B CN 106192212B
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- cnfs
- woven fabrics
- carbon fiber
- confinement
- fiber mesh
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Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/002—Inorganic yarns or filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
Abstract
The present invention relates to a kind of preparation methods of nano-cellulose based carbon fiber mesh non-woven fabrics electrode.The present invention uses numerical control wet-spinning techniques, nano-cellulose (CNFs) spinning solution containing catalytic dehydrating agent is first woven into CNFs grid cloths, then CNFs grid non-woven fabrics is prepared using confinement dry technology, CNFs based carbon fiber mesh non-woven fabrics flexible electrode materials is prepared finally by pre-oxidation, carbonization and using confinement technology.The CNFs based carbon fiber mesh non-woven fabrics flexible electrode materials prepared by foregoing invention method have the characteristics that the generation of no off-line phenomenon, latitude and longitude intersection are mutually merged, flexibility is good, thickness is thin, good conductivity；Its thickness is 0.10 0.14mm；Square resistance is 30.68 60.18 Ω/.
Description
Technical field
The present invention relates to a kind of carbon fiber mesh non-woven fabrics flexible electrode material more particularly to a kind of nano-cellulose base carbon
The preparation method of fiber mesh non-woven fabrics flexible electrode material, belongs to flexible electrode material field.
Background technology
Carbon cloth is also carbon fiber woven cloth, is that carbon fiber is prepared by knitting skill.Carbon cloth has
The advantages that intensity is high, density is small, thickness is thin and satisfactory electrical conductivity.Therefore, carbon cloth is usually used to preparation structure material.
These carbon cloth based structures materials are widely applied in fields such as aerospace, industry, sports equipment and buildings.
Preferable electric conductivity, it is flexible the features such as make carbon cloth that there is wide application in flexible energy device field before
Scape.Thus carbon cloth is just applied and conducts in-depth research work in flexible energy device field by people in recent years, and takes
Obtained certain progress.However, traditional carbon fibres cloth is usually to be woven by carbon fiber.This weaving carbon fiber cloth not only exists
Edge is prone to off-line phenomenon, and there is bigger contact resistances for latitude and longitude intersection, this does not utilize tradition
Extensive use of the carbon cloth in flexible energy device field.
It will found in cellulosic material nanosizing research process, utilizing 2,2,6,6- tetramethyl piperidine -1- oxygroups
(TEMPO) nano-cellulose (CNFs) prepared by catalytic oxidation has good wet spinning, using numerical control wet-spinning techniques, leads to
The thread-off prevention line nano-cellulose grid non-woven fabrics mutually merged latitude and longitude intersection can be prepared by crossing confinement drying, after carbonization just
The thread-off prevention line carbon fiber mesh non-woven fabrics of contact resistance disappearance can directly be prepared.
The present invention uses numerical control wet-spinning techniques, CNFs spinning solutions is first woven into CNFs grid cloths in freezing solidly on, so
CNFs grid non-woven fabrics is prepared using confinement dry technology afterwards, it is finally by pre-oxidation, carbonization and direct using confinement technology
Prepare CNFs based carbon fiber mesh non-woven fabrics.The CNFs based carbon fiber mesh non-woven fabrics latitude and longitude prepared by above-mentioned technique
It mutually merges intersection.This not only can fundamentally prevent the generation of off-line phenomenon, but also can make latitude and longitude contact resistance
It disappears.This is beneficial to CNFs based carbon fiber mesh non-woven fabrics and is used widely in flexible energy device field.
Invention content
The present invention is prone to off-line to simplify traditional carbon fibres cloth preparation process, solve traditional carbon fibres cloth edge
The problems such as there are contact resistances phenomenon and latitude and longitude intersection, and a kind of nano-cellulose based carbon fiber mesh non-woven fabrics is provided
The preparation method of flexible electrode material.
The purpose of the present invention is what is realized by following technical proposals：
A kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, is as follows：
Step 1: different types of cellulosic material (wood pulp, bamboo pulp, cotton pulp) utilizes TEMPO catalysis oxidations, ultrasound point
Dissipate, vacuum rotating concentration and etc. be prepared CNFs suspension, wherein the mass fraction of CNFs is 0.5%~1.2%；
Step 2: a certain amount of variety classes catalytic dehydrating agent is added in the obtained CNFs suspension of step 1, it is acute
10~60min of strong stirring, 5~60min of froth in vacuum obtain CNFs spinning solutions.
Step 3: the obtained CNFs spinning solutions of 30ml step 2 are injected into the syringe of 50ml.Using micro
Syringe pump control CNFs spinning solutions are entered with certain flow (2.5-5.5ml/h) by the tack syringe needle that internal diameter is 0.41mm solidifying
Gu in bath.Wherein CNFs grids non-woven fabrics size and braiding structure control the movement braiding of tack syringe needle by using numerical control device
Strategy is realized.CNFs grid cloths aging 30min in coagulating bath after the completion of braiding.
Step 4: the obtained CNFs grid cloths of step 3 are dried 1~6h under the conditions of 30~100 DEG C, confinement.It prepares
Go out dry state CNFs grid non-woven fabrics.
Step 5: the obtained dry state CNFs grids non-woven fabrics of step 4 is each pre- under confinement and specific temperature conditions
Aoxidize 30min.Obtain pre-oxidation CNFs grid non-woven fabrics.
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 in confinement, different atmosphere, specific temperature item
It is carbonized certain time under part.Obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Variety classes catalytic dehydrating agent described in step 2 includes NH4H2PO4、(NH4)2HPO4、NH4HSO4(NH4)2SO4, thiocarbamide and urea etc..
The catalytic dehydrating agent percentage composition (catalytic dehydrating agent/(catalytic dehydrating agent+CNFs)) being added in step 2 be 5%~
20%.
Confinement condition is 2D confinement conditions in step 4, i.e., generates a 2D tension environment in the drying process.
Confinement condition is 2D confinement conditions in step 5, i.e., a 2D tension environment is generated in preoxidation process.
Specific temperature is 120,165,210,230,250,270,290,310 DEG C in step 5.
Confinement condition is 2D confinement conditions in step 6, i.e., a 2D tension environment is generated in carbonisation.
Different atmosphere is N in step 62, Ar and Ar+H2Gaseous mixture.
Specific temperature is 600 DEG C, 1100 DEG C in step 6.
Carbonization time is 30~60min in step 6.
Advantageous effect
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material of the present invention, grid
Latitude and longitude intersection is mutually merged in non-woven fabrics, has fundamentally been prevented the generation of off-line phenomenon and has been realized latitude and longitude contact
The disappearance of resistance.Thus, the nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material being prepared by this method
With good conductive, mechanical flexibility energy.
Prevent to take off 2. the nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material made from this method has
The features such as generation of line phenomenon, latitude and longitude intersection are mutually merged, flexibility is good, thickness is thin, good conductivity；Its flexibility is good
It is good；Thickness is 0.10-0.14mm；Square resistance is 30.68-60.18 Ω/；
Description of the drawings
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material pictorial diagram obtained when attached drawing 1 is condition 1.
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material flexibility exhibition obtained when attached drawing 2 is condition 1
Diagram.
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude phase obtained when attached drawing 3 is condition 1
SEM schemes at friendship.
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude phase obtained when attached drawing 4 is condition 2
SEM schemes at friendship.
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude phase obtained when attached drawing 5 is condition 3
SEM schemes at friendship.
Nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude phase obtained when attached drawing 6 is condition 4
SEM schemes at friendship.
Specific implementation mode
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, specific steps are such as
Under：
Step 1: wood pulp using TEMPO catalysis oxidations, ultrasonic disperse, vacuum rotating concentrate and etc. CNFs is prepared
Suspension, the wherein mass fraction of CNFs are 0.7%；
Step 2: by (NH4)2HPO4Catalytic dehydrating agent (10% content) is added to the obtained CNFs suspension of step 1
In, it is vigorously stirred 30min, froth in vacuum 60min obtains CNFs spinning solutions；
Step 3: the obtained CNFs spinning solutions of 20ml step 2 are injected into the syringe of 50ml specifications.It utilizes
Micro-injection pump control CNFs spinning solutions enter coagulating bath by internal diameter with the flow of 4.5ml/h for the tack syringe needle of 0.41mm
In.Wherein CNFs grids non-woven fabrics size and braiding structure control the movement weaving strategy of tack syringe needle by using numerical control device
To realize.CNFs grid cloths aging 30min in coagulating bath after the completion of braiding；
Step 4: the obtained CNFs grids non-woven fabrics of step 3 is dried 2h under the conditions of 60 DEG C, confinement.It prepares dry
State CNFs grid non-woven fabrics；
Step 5: by the obtained dry state CNFs grids non-woven fabrics of step 4 in confinement condition, 120 DEG C, 165 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, respectively pre-oxidize 30min at 310 DEG C.Obtain pre-oxidation CNFs grid non-woven fabrics.
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 in confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of 60min that are carbonized respectively.Obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Obtained nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude intersection mutually merges,
Flexibility is good；Thickness is 0.10mm；Square resistance is 30.68 Ω/.
Embodiment 2
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, specific steps are such as
Under：
Step 1: bamboo pulp using TEMPO catalysis oxidations, ultrasonic disperse, vacuum rotating concentrate and etc. CNFs is prepared
Suspension, the wherein mass fraction of CNFs are 0.65%；
Step 2: by NH4H2PO4Catalytic dehydrating agent (15% content) is added in the obtained CNFs suspension of step 1,
It is vigorously stirred 40min, froth in vacuum 60min obtains CNFs spinning solutions；
Step 3: the obtained CNFs spinning solutions of 20ml step 2 are injected into the syringe of 50ml specifications.It utilizes
Micro-injection pump control CNFs spinning solutions enter coagulating bath by internal diameter with the flow of 5.1ml/h for the tack syringe needle of 0.41mm
In.Wherein CNFs grids non-woven fabrics size and braiding structure control the movement weaving strategy of tack syringe needle by using numerical control device
To realize.CNFs grid cloths aging 30min in coagulating bath after the completion of braiding；
Step 4: the obtained CNFs grid cloths of step 3 are dried 2h under the conditions of 60 DEG C, confinement.Prepare dry state
CNFs grid non-woven fabrics；
Step 5: by the obtained dry state CNFs grids non-woven fabrics of step 4 in confinement condition, 120 DEG C, 165 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, respectively pre-oxidize 30min at 310 DEG C.Obtain pre-oxidation CNFs grid non-woven fabrics.
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 in confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of 60min that are carbonized respectively.Obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Obtained nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude intersection mutually merges,
Flexibility is good；Thickness is 0.14mm；Square resistance is 39.56 Ω/.
Embodiment 3
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, specific steps are such as
Under：
Step 1: cotton pulp using TEMPO catalysis oxidations, ultrasonic disperse, vacuum rotating concentrate and etc. CNFs is prepared
Suspension, the wherein mass fraction of CNFs are 0.75%；
Step 2: by NH4H2PO4+(NH4)2HPO4Catalytic dehydrating agent (12% content NH4H2PO4/(NH4)2HPO4=1/1)
It is added in the obtained CNFs suspension of step 1, is vigorously stirred 40min, froth in vacuum 60min obtains CNFs spinning solutions；
Step 3: the obtained CNFs spinning solutions of 20ml step 2 are injected into the syringe of 50ml specifications.It utilizes
Micro-injection pump control CNFs spinning solutions enter coagulating bath by internal diameter with the flow of 4.5ml/h for the tack syringe needle of 0.41mm
In.Wherein CNFs grids non-woven fabrics size and braiding structure control the movement weaving strategy of tack syringe needle by using numerical control device
To realize.CNFs grid cloths aging 30min in coagulating bath after the completion of braiding；
Step 4: the obtained CNFs grid cloths of step 3 are dried 2h under the conditions of 60 DEG C, confinement.Prepare dry state
CNFs grid non-woven fabrics；
Step 5: by the obtained dry state CNFs grids non-woven fabrics of step 4 in confinement condition, 120 DEG C, 165 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, respectively pre-oxidize 30min at 310 DEG C.Obtain pre-oxidation CNFs grid non-woven fabrics.
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 in confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of 60min that are carbonized respectively.Obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Obtained nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude intersection mutually merges,
Flexibility is good；Thickness is 0.10mm；Square resistance is 46.21 Ω/.
Embodiment 4
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, specific steps are such as
Under：
Step 1: wood pulp using TEMPO catalysis oxidations, ultrasonic disperse, vacuum rotating concentrate and etc. CNFs is prepared
Suspension, the wherein mass fraction of CNFs are 0.67%；
Step 2: by (NH4)2HPO4Catalytic dehydrating agent (12% content NH4H2PO4/(NH4)2HPO4=1/1) it is added to step
In a rapid obtained CNFs suspension, it is vigorously stirred 40min, froth in vacuum 60min obtains CNFs spinning solutions；
Step 3: the obtained CNFs spinning solutions of 20ml step 2 are injected into the syringe of 50ml specifications.It utilizes
Micro-injection pump control CNFs spinning solutions enter coagulating bath by internal diameter with the flow of 4.9ml/h for the tack syringe needle of 0.41mm
In.Wherein CNFs grids non-woven fabrics size and braiding structure control the movement weaving strategy of tack syringe needle by using numerical control device
To realize.CNFs grid cloths aging 30min in coagulating bath after the completion of braiding；
Step 4: the obtained CNFs grid cloths of step 3 are dried 2h under the conditions of 60 DEG C, confinement.Prepare dry state
CNFs grid non-woven fabrics；
Step 5: by the obtained dry state CNFs grids non-woven fabrics of step 4 in confinement condition, 120 DEG C, 165 DEG C, 210
DEG C, 230 DEG C, 250 DEG C, 270 DEG C, 290 DEG C, respectively pre-oxidize 30min at 310 DEG C.Obtain pre-oxidation CNFs grid non-woven fabrics.
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 in confinement condition, Ar atmosphere, 600 DEG C,
1100 DEG C of 60min that are carbonized respectively.Obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Obtained nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material latitude and longitude intersection mutually merges,
Flexibility is good；Thickness is 0.14mm；Square resistance is 60.18 Ω/.
Claims (5)
1. a kind of preparation method of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode, including steps are as follows：
Step 1: cellulosic material wood pulp, bamboo pulp or cotton pulp are concentrated using TEMPO catalysis oxidations, ultrasonic disperse, vacuum rotating
The step of be prepared CNFs suspension, the mass fraction of CNFs is 0.5%-1.2% in the CNFs suspension；
Step 2: a certain amount of catalytic dehydrating agent is added in the obtained CNFs suspension of step 1, it is vigorously stirred 10-
60min, froth in vacuum 5-60min obtain CNFs spinning solutions；The catalytic dehydrating agent is NH4H2PO4、(NH4)2HPO4、
NH4HSO4Or (NH4)2SO4；
Step 3: the obtained CNFs spinning solutions of 30mL step 2 are injected into the syringe of 50mL, micro-injection is utilized
Pump control CNFs spinning solutions are that 2.5-5.5mL/h is entered for the tack syringe needle of 0.41mm in coagulating bath by internal diameter with flow,
And the movement weaving strategy of tack syringe needle is controlled by numerical control device and is sized and braiding structure CNFs grids to obtain having
Non-woven fabrics, CNFs grid non-woven fabrics aging 30min in coagulating bath after the completion of weaving；
Step 4: the obtained CNFs grids non-woven fabrics of step 3 is dried 1-6h under the conditions of 30-100 DEG C, confinement, prepare
Dry state CNFs grid non-woven fabrics；
Step 5: by the obtained dry state CNFs grids non-woven fabrics of step 4 under the conditions of confinement, 120,165,210,230,
250,30min is respectively pre-oxidized under 270,290,310 DEG C of temperature conditions, obtains pre-oxidation CNFs grid non-woven fabrics；
Step 6: by the obtained pre-oxidation CNFs grids non-woven fabrics of step 5 under the conditions of confinement, in N2, Ar or Ar+H2Mixing
In gas atmosphere, be carbonized 30~60min respectively under 600 DEG C and 1100 DEG C of temperature conditions, obtains nano-cellulose based carbon fiber mesh
Non-woven fabrics flexible electrode material.
2. preparation method according to claim 1, which is characterized in that it is de- that the catalytic dehydrating agent being added in step 2 accounts for catalysis
Aqua and the mass percentage of CNFs quality sums are 5%~20%.
3. preparation method according to claim 1, which is characterized in that confinement condition is to produce in the drying process in step 4
A raw 2D tension environment.
4. preparation method according to claim 1, which is characterized in that confinement condition is in preoxidation process in step 5
Generate a 2D tension environment.
5. preparation method according to claim 1, which is characterized in that confinement condition is to be produced in carbonisation in step 6
A raw 2D tension environment.
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| CN109440228B (en) * | 2018-11-07 | 2021-05-18 | 武汉轻工大学 | Preparation method of cellulose-based carbon nanofiber |
| CN109440212B (en) * | 2018-11-28 | 2021-05-11 | 五邑大学 | Preparation method of high-orientation high-toughness regenerated cellulose fiber and high-orientation high-toughness regenerated cellulose fiber |
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