CN106192212A - 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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- CN106192212A CN106192212A CN201610542494.5A CN201610542494A CN106192212A CN 106192212 A CN106192212 A CN 106192212A CN 201610542494 A CN201610542494 A CN 201610542494A CN 106192212 A CN106192212 A CN 106192212A
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- cnfs
- woven fabrics
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- carbon fiber
- confinement
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Classifications
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- 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 the preparation method of a kind of nano-cellulose based carbon fiber mesh non-woven fabrics electrode.The present invention uses numerical control wet-spinning techniques, first nano-cellulose (CNFs) spinning solution containing catalytic dehydrating agent is woven into CNFs grid cloth, then confinement dry technology is utilized to prepare CNFs grid non-woven fabrics, finally by pre-oxidation, carbonization utilize confinement technology to prepare CNFs based carbon fiber mesh non-woven fabrics flexible electrode material.The CNFs based carbon fiber mesh non-woven fabrics flexible electrode material prepared by foregoing invention method have the generation without off-line phenomenon, mutually merge through parallel intersection, the feature such as pliability 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, particularly relate 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
Intensity is high, density is little, thickness is thin and the advantage such as satisfactory electrical conductivity.Therefore, carbon cloth is usually used to prepare structural material.
These carbon cloth based structures materials are widely applied in fields such as aerospace, industry, sports equipment and buildings.
Preferably electric conductivity, the feature such as pliable and tough makes carbon cloth before flexible energy device field has wide application
Scape.Thus carbon cloth is just applied and expanded in-depth study work in flexible energy device field by people in recent years, and take
Obtained certain progress.But, traditional carbon fibres cloth is usually and is formed by carbon fiber braiding.This weaving carbon fiber cloth not only exists
Edge is prone to off-line phenomenon, and there is bigger contact resistance through parallel intersection, and this does not the most utilize tradition
The carbon cloth extensive application in flexible energy device field.
By cellulosic material nanorize research process finds, utilize 2,2,6,6-tetramethyl piperidine-1-epoxides
(TEMPO) nano-cellulose (CNFs) that prepared by catalytic oxidation has good wet spinning, utilizes numerical control wet-spinning techniques, logical
Cross confinement to be dried and can prepare the anti-off-line nano-cellulose grid non-woven fabrics mutually merged through parallel intersection, after carbonization just
Can directly prepare the anti-off-line carbon fiber mesh non-woven fabrics that contact resistance disappears.
The present invention uses numerical control wet-spinning techniques, first CNFs spinning solution is woven in freezing solidly on CNFs grid cloth, so
After utilize confinement dry technology to prepare CNFs grid non-woven fabrics, finally by pre-oxidation, carbonization utilize confinement technology direct
Prepare CNFs based carbon fiber mesh non-woven fabrics.The CNFs based carbon fiber mesh non-woven fabrics prepared by above-mentioned technique is through parallel
Intersection is mutually merged.This generation being possible not only to fundamentally stop off-line phenomenon, and longitude and latitude linear contact lay resistance can be made
Disappear.This is beneficial to CNFs based carbon fiber mesh non-woven fabrics and is used widely in flexible energy device field.
Summary of the invention
The present invention is in order to simplify traditional carbon fibres cloth preparation technology, solve traditional carbon fibres cloth edge and be prone to off-line
Phenomenon and there is the problems such as contact resistance through parallel intersection, and a kind of nano-cellulose based carbon fiber mesh non-woven fabrics is provided
The preparation method of flexible electrode material.
It is an object of the invention to be realized by following technical proposals:
The preparation method of a kind of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, specifically comprises the following steps that
Step one, different types of cellulosic material (wood pulp, bamboo pulp, cotton pulp) utilize TEMPO catalysis oxidation, ultrasonic point
The steps such as scattered, vacuum rotating concentration prepare CNFs suspension, and wherein the mass fraction of CNFs is 0.5%~1.2%;
Step 2, a certain amount of variety classes catalytic dehydrating agent is joined in the CNFs suspension obtained by step one, acute
Strong stirring 10~60min, froth in vacuum 5~60min obtain CNFs spinning solution.
Step 3, the CNFs spinning solution obtained by 30ml step 2 is injected in the syringe of 50ml.Utilize trace
Syringe pump is controlled CNFs spinning solution and is entered by the internal diameter tack syringe needle as 0.41mm with certain flow (2.5-5.5ml/h) and coagulate
Gu in Yu.The motion that wherein CNFs grid non-woven fabrics size and braiding structure control tack syringe needle by utilizing numerical control device weaves
Strategy realizes.Weave rear CNFs grid cloth aging 30min in coagulating bath.
Step 4, by the CNFs grid cloth obtained by step 3 30~100 DEG C, be dried 1~6h under the conditions of confinement.Preparation
Go out dry state CNFs grid non-woven fabrics.
Step 5, by the dry state CNFs grid non-woven fabrics obtained by step 4 under confinement and specific temperature conditions each pre-
Oxidation 30min.Obtain pre-oxidizing CNFs grid non-woven fabrics.
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 at confinement, different atmosphere, specified temp bar
Carbonization 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, thiourea and carbamide etc..
In step 2 add catalytic dehydrating agent percentage composition (catalytic dehydrating agent/(catalytic dehydrating agent+CNFs)) be 5%~
20%.
In step 4, confinement condition is 2D confinement condition, i.e. produces a 2D tension force environment in dry run.
In step 5, confinement condition is 2D confinement condition, i.e. produces a 2D tension force environment in preoxidation process.
In step 5, specified temp is 120,165,210,230,250,270,290,310 DEG C.
In step 6, confinement condition is 2D confinement condition, i.e. produces a 2D tension force environment in carbonisation.
In step 6, different atmosphere is N2, Ar and Ar+H2Gaseous mixture.
In step 6, specified temp is 600 DEG C, 1100 DEG C.
In step 6, carbonization time is 30~60min.
Beneficial effect
1. the preparation method of a kind of nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material of the present invention, grid
Non-woven fabrics mutually merges through parallel intersection, has fundamentally stopped the generation of off-line phenomenon and achieved longitude and latitude linear contact lay
The disappearance of resistance.Thus, the nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared by this method
There is good conduction, mechanical flexibility energy.
2. the nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared by this method has have been stopped to take off
The generation of line phenomenon, mutually merge through parallel intersection, the feature such as pliability is good, thickness is thin, good conductivity;Its pliability is good
Good;Thickness is 0.10-0.14mm;Square resistance is 30.68-60.18 Ω/;
Accompanying drawing explanation
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material pictorial diagram prepared when accompanying drawing 1 is condition 1.
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material pliability exhibition prepared when accompanying drawing 2 is condition 1
Diagram.
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared when accompanying drawing 3 is condition 1 is through parallel phase
SEM figure at friendship.
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared when accompanying drawing 4 is condition 2 is through parallel phase
SEM figure at friendship.
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared when accompanying drawing 5 is condition 3 is through parallel phase
SEM figure at friendship.
The nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material prepared when accompanying drawing 6 is condition 4 is through parallel phase
SEM figure at friendship.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
1. a preparation method for nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, concrete steps are such as
Under:
Step one, wood pulp utilize the steps such as TEMPO catalysis oxidation, ultrasonic disperse, vacuum rotating concentration to prepare CNFs
Suspension, wherein the mass fraction of CNFs is 0.7%;
Step 2, by (NH4)2HPO4Catalytic dehydrating agent (10% content) joins the CNFs suspension obtained by step one
In, it is stirred vigorously 30min, froth in vacuum 60min obtains CNFs spinning solution;
Step 3, the CNFs spinning solution obtained by 20ml step 2 is injected in the syringe of 50ml specification.Utilize
Micro-injection pump control CNFs spinning solution passes through the internal diameter tack syringe needle entrance coagulating bath as 0.41mm with the flow of 4.5ml/h
In.Wherein CNFs grid non-woven fabrics size and braiding structure are by utilizing numerical control device to control the motion weaving strategy of tack syringe needle
Realize.Weave rear CNFs grid cloth aging 30min in coagulating bath;
Step 4, by the CNFs grid non-woven fabrics obtained by step 3 60 DEG C, be dried 2h under the conditions of confinement.Prepare dry
State CNFs grid non-woven fabrics;
Step 5, by the dry state CNFs grid non-woven fabrics obtained by 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-oxidizing CNFs grid non-woven fabrics.
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 at confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of respectively carbonization 60min.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 mutually merges through parallel intersection,
Pliability is good;Thickness is 0.10mm;Square resistance is for for 30.68 Ω/.
Embodiment 2
1. a preparation method for nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, concrete steps are such as
Under:
Step one, bamboo pulp utilize the steps such as TEMPO catalysis oxidation, ultrasonic disperse, vacuum rotating concentration to prepare CNFs
Suspension, wherein the mass fraction of CNFs is 0.65%;
Step 2, by NH4H2PO4Catalytic dehydrating agent (15% content) joins in the CNFs suspension obtained by step one,
Be stirred vigorously 40min, froth in vacuum 60min obtains CNFs spinning solution;
Step 3, the CNFs spinning solution obtained by 20ml step 2 is injected in the syringe of 50ml specification.Utilize
Micro-injection pump control CNFs spinning solution passes through the internal diameter tack syringe needle entrance coagulating bath as 0.41mm with the flow of 5.1ml/h
In.Wherein CNFs grid non-woven fabrics size and braiding structure are by utilizing numerical control device to control the motion weaving strategy of tack syringe needle
Realize.Weave rear CNFs grid cloth aging 30min in coagulating bath;
Step 4, by the CNFs grid cloth obtained by step 3 60 DEG C, be dried 2h under the conditions of confinement.Prepare dry state
CNFs grid non-woven fabrics;
Step 5, by the dry state CNFs grid non-woven fabrics obtained by 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-oxidizing CNFs grid non-woven fabrics.
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 at confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of respectively carbonization 60min.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 mutually merges through parallel intersection,
Pliability is good;Thickness is 0.14mm;Square resistance is for for 39.56 Ω/.
Embodiment 3
1. a preparation method for nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, concrete steps are such as
Under:
Step one, cotton pulp utilize the steps such as TEMPO catalysis oxidation, ultrasonic disperse, vacuum rotating concentration to prepare CNFs
Suspension, wherein the mass fraction of CNFs is 0.75%;
Step 2, by NH4H2PO4+(NH4)2HPO4Catalytic dehydrating agent (12% content NH4H2PO4/(NH4)2HPO4=1/1)
Join in the CNFs suspension obtained by step one, be stirred vigorously 40min, froth in vacuum 60min obtains CNFs spinning solution;
Step 3, the CNFs spinning solution obtained by 20ml step 2 is injected in the syringe of 50ml specification.Utilize
Micro-injection pump control CNFs spinning solution passes through the internal diameter tack syringe needle entrance coagulating bath as 0.41mm with the flow of 4.5ml/h
In.Wherein CNFs grid non-woven fabrics size and braiding structure are by utilizing numerical control device to control the motion weaving strategy of tack syringe needle
Realize.Weave rear CNFs grid cloth aging 30min in coagulating bath;
Step 4, by the CNFs grid cloth obtained by step 3 60 DEG C, be dried 2h under the conditions of confinement.Prepare dry state
CNFs grid non-woven fabrics;
Step 5, by the dry state CNFs grid non-woven fabrics obtained by 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-oxidizing CNFs grid non-woven fabrics.
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 at confinement condition, Ar+H2Atmosphere, 600
DEG C, 1100 DEG C of respectively carbonization 60min.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 mutually merges through parallel intersection,
Pliability is good;Thickness is 0.10mm;Square resistance is for for 46.21 Ω/.
Embodiment 4
1. a preparation method for nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material, concrete steps are such as
Under:
Step one, wood pulp utilize the steps such as TEMPO catalysis oxidation, ultrasonic disperse, vacuum rotating concentration to prepare CNFs
Suspension, wherein the mass fraction of CNFs is 0.67%;
Step 2, by (NH4)2HPO4Catalytic dehydrating agent (12% content NH4H2PO4/(NH4)2HPO4=1/1) step is joined
In CNFs suspension obtained by rapid one, be stirred vigorously 40min, froth in vacuum 60min obtains CNFs spinning solution;
Step 3, the CNFs spinning solution obtained by 20ml step 2 is injected in the syringe of 50ml specification.Utilize
Micro-injection pump control CNFs spinning solution passes through the internal diameter tack syringe needle entrance coagulating bath as 0.41mm with the flow of 4.9ml/h
In.Wherein CNFs grid non-woven fabrics size and braiding structure are by utilizing numerical control device to control the motion weaving strategy of tack syringe needle
Realize.Weave rear CNFs grid cloth aging 30min in coagulating bath;
Step 4, by the CNFs grid cloth obtained by step 3 60 DEG C, be dried 2h under the conditions of confinement.Prepare dry state
CNFs grid non-woven fabrics;
Step 5, by the dry state CNFs grid non-woven fabrics obtained by 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-oxidizing CNFs grid non-woven fabrics.
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 in confinement condition, Ar atmosphere, 600 DEG C,
1100 DEG C of difference carbonization 60min.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 mutually merges through parallel intersection,
Pliability is good;Thickness is 0.14mm;Square resistance is for for 60.18 Ω/.
Claims (10)
1. a preparation method for nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode, comprises the following steps that
Step one, different types of cellulosic material (wood pulp, bamboo pulp, cotton pulp) utilize TEMPO catalysis oxidation, ultrasonic disperse, very
The steps such as empty spin concentration prepare CNFs suspension, and wherein the mass fraction of CNFs is 0.5%~1.2%;
Step 2, a certain amount of variety classes catalytic dehydrating agent is joined in the CNFs suspension obtained by step one, acutely stir
Mix 10~60min, froth in vacuum 5~60min obtains CNFs spinning solution;
Step 3, the CNFs spinning solution obtained by 30ml step 2 is injected in the syringe of 50ml, utilizes micro-injection
Pump control CNFs spinning solution with certain flow (2.5-5.5ml/h) by internal diameter as 0.41mm tack syringe needle entrance coagulating bath
In, wherein CNFs grid non-woven fabrics size and braiding structure are by utilizing numerical control device to control the motion weaving strategy of tack syringe needle
Realize, woven rear CNFs grid cloth aging 30min in coagulating bath;
Step 4, by the CNFs grid cloth obtained by step 3 30~100 DEG C, be dried 1~6h under the conditions of confinement, prepare dry
State CNFs grid non-woven fabrics;
Step 5, the dry state CNFs grid non-woven fabrics obtained by step 4 is respectively pre-oxidized under confinement and specific temperature conditions
30min, obtains pre-oxidizing CNFs grid non-woven fabrics;
Step 6, by the pre-oxidation CNFs grid non-woven fabrics obtained by step 5 in confinement, different atmosphere, under specific temperature conditions
Carbonization certain time, obtain nano-cellulose based carbon fiber mesh non-woven fabrics flexible electrode material.
Preparation method the most according to claim 1, it is characterised in that the variety classes catalytic dehydrating agent described in step 2
Including NH4H2PO4、(NH4)2HPO4、NH4HSO4(NH4)2SO4, thiourea and carbamide etc..
Preparation method the most according to claim 1, it is characterised in that the catalytic dehydrating agent percentage composition added in step 2
(catalytic dehydrating agent/(catalytic dehydrating agent+CNFs)) is 5%~20%.
Preparation method the most according to claim 1, it is characterised in that in step 4, confinement condition is 2D confinement condition, i.e.
A 2D tension force environment is produced in dry run.
Preparation method the most according to claim 1, it is characterised in that in step 5, confinement condition is 2D confinement condition, i.e.
A 2D tension force environment is produced in preoxidation process.
Preparation method the most according to claim 1, it is characterised in that in step 5 specified temp be 120,165,210,
230、250、270、290、310℃。
Preparation method the most according to claim 1, it is characterised in that in step 6, confinement condition is 2D confinement condition, i.e.
A 2D tension force environment is produced in carbonisation.
Preparation method the most according to claim 1, it is characterised in that in step 6, different atmosphere is N2, Ar and Ar+H2
Gaseous mixture.
Preparation method the most according to claim 1, it is characterised in that in step 6, specified temp is 600 DEG C, 1100 DEG C.
Preparation method the most according to claim 1, it is characterised in that in step 6, carbonization time is 30~60min.
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CN109440212A (en) * | 2018-11-28 | 2019-03-08 | 五邑大学 | The preparation method of the highly oriented tough regenerated celulose fibre of height and the highly oriented tough regenerated celulose fibre of height |
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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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