CN107022810A - A kind of amine based polymer composite graphite alkene height leads fiber and preparation method thereof - Google Patents
A kind of amine based polymer composite graphite alkene height leads fiber and preparation method thereof Download PDFInfo
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- CN107022810A CN107022810A CN201710310327.2A CN201710310327A CN107022810A CN 107022810 A CN107022810 A CN 107022810A CN 201710310327 A CN201710310327 A CN 201710310327A CN 107022810 A CN107022810 A CN 107022810A
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- graphene oxide
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- 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
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- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
Fiber and preparation method thereof is led the invention discloses a kind of amine based polymer composite graphite alkene height, by the graphene oxide activation process that mass fraction is 1~10%, it is compound with amine based polymer, resulting solution from spinning nozzle be expressed into coagulating bath in obtain graphene oxide composite fibre.Gained graphene oxide composite fibre obtains graphene composite fibre further across reduction.The graphene composite fibre of gained has very high conductance and modulus, and fracture strength is more than 1.6cN/tex, and conductance is more than 9.2S/cm.Graphene composite fibre prepared by the present invention has excellent electric conductivity and mechanical property, is expected to be used for lightweight wire, ultralight electric wire.
Description
Technical field
The present invention relates to a kind of fiber based on graphene, especially a kind of graphene composite fibre with high conductivity
And preparation method thereof.
Background technology
Graphene possesses the physical and chemical properties such as very excellent and unique light, electricity, heat, the heat as Recent study
Point.From practical standpoint consider, graphene macroscopic material, such as gel, film, foam, fiber form, flexible electronic device,
The fields such as energy storage, sensing show huge application prospect.
Wherein, graphene fiber has good electric conductivity and mechanical property, while there is high pliability and processability,
So that the preparation and application of graphene fiber have obtained widely studied.At present, domestic and international a few studies person is respectively by different
Method has prepared graphene fiber.But often there is the shortcomings of intensity is relatively low, fragility is larger in pure graphene fiber, therefore,
Generally graphene fiber is modified by adding the method for polymer.For example, in patent CN104451925A, will be water-soluble
Property the blending of polymer and graphene oxide prepare spinning solution, then carry out wet spinning, gained graphene composite fibre intensity is big
In 100MPa, elongation at break is more than 2%, but its electrical conductivity is more than 0.1S/cm.And for example in patent CN102181961B, by graphite
Wet spinning after the blending of alkene and sodium alginate, obtains the composite fibre with higher-strength, but be wherein graphene addition very
It is low（＜ 15%）, the electric conductivity of composite fibre is low.The modified graphene fiber reported at present is substantially all by the side of physical blending
Method is realized, the graphene fiber that prepare high intensity can be modified by the method for Chemical Physics, empty with very big development
Between.
The content of the invention
In view of the shortcomings of the prior art, the present invention proposes a kind of preparation method that composite fibre is led based on graphene height.
The technical proposal for solving the technical problem of the invention is：By graphene oxide activation process, with amino-contained
Polymer be combined, resulting solution from spinning nozzle be expressed into coagulating bath in obtain graphene oxide composite fibre；Again by chemistry also
Original, obtains super High conductivity graphene composite fibre.Described composite fibre mainly includes following component：In parts by weight, 1 weight
Measure the graphene oxide of part, the activator of 0.001~0.01 parts by weight, the amine based polymer of 0.01~0.2 parts by weight, 0.5~5
The reducing agent of parts by weight.
Described graphene oxide be graphite by pre-oxidation, peel off, oxidation, filtering, washing, dry after obtain
Graphene oxide, is at least one of graphene oxide, carboxylated graphene oxide, sulfonic group graphene oxide.
Described activator mainly includes 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, dicyclohexyl
It is one or more kinds of according to any proportioning mixing composition in carbodiimide, BTA base diethyl phosphate.
Described amine based polymer mainly include polyacrylamide, polycaprolactam, poly- N, N '-N-isopropylacrylamide,
One kind in polyhexamethylene adipamide, polydecamethylene adipamide, polyaniline, chitosan, fibroin albumen etc..
Described coagulating bath is by one kind in acetic acid, ethyl acetate, butyl acetate, methanol, ethanol, glycerine, acetone etc.
Or it is a variety of according to any proportioning mixing composition.
Described reducing agent mainly includes sodium hydrogensulfite, hydroiodic acid, glucose, hydrazine hydrate, sodium borohydride, vitamin C
At least one of.
A kind of amine based polymer composite graphite alkene height leads the preparation method of fiber, and the preparation method mainly includes following step
Suddenly：In the solvent that the graphene oxide of 1 parts by weight is dissolved in 10~100 parts by weight, it is ultrasonically treated after obtain finely dispersed
Graphene oxide solution, then add 0.001~0.01 parts by weight activator, activation 10~120min after add 0.01~
5~60min of ultrasound after the polymer of the amino-contained of 0.2 parts by weight, 6~48h of reaction, squeezing with 1~30mL/h after being uniformly dispersed
Go out speed, after being extruded by aperture spinneret, into coagulating bath, 10~100s is stopped in 10~60 DEG C of coagulating bath, with red
Outer lamp is dried, and obtains graphene oxide composite fibre, is finally placed in 50~90 DEG C of 5~480min of reduction in reducing agent, and washing is dry
It is dry, it just can obtain graphene composite fibre.
The beneficial effects of the invention are as follows：Compared with prior art, graphene composite fibre of the invention has higher strong
Degree and good electric conductivity, compensate for the fragility of pure graphene fiber；Even structure, is provided for the serialization of graphene fiber
It is convenient；Composite fibre, using micro Treatment with activating agent, is chemically bonded during preparation with the polymer of amino-contained
Effect, improves the continuity of fiber, the composition and performance of convenient regulation composite fibre；In addition, the compound fibre of the graphene of the present invention
Dimension table face has groove microstructure, with good electric conductivity and thermal conductivity, antistatic and conductive fabric, electro-magnetic wave absorption with
The fields such as loomage, sensor and water process are with a wide range of applications.
Brief description of the drawings
Fig. 1 is the graphene composite fibre heavy burden 5g counterweight digital photographs of 10 days that prepare in embodiment 1.
Fig. 2 is the microphotograph of the graphene composite fibre prepared in embodiment 1.
Fig. 3 is the control group graphene fiber heavy burden 5g counterweight digital photographs of 10 days.
Embodiment
The present invention is further illustrated below by specific embodiment.But these examples be merely to illustrate the present invention and without
In limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, conventionally and condition, or
Selected according to catalogue.
In following embodiments, graphene oxide is prepared according to Hummers oxidizing process, and the average grain diameter of graphite used is
30 μm, other raw materials are commercially available.The diameter of graphene composite fibre is obtained by optical microscope measuring；Tensile strength,
Elongation at break is tested by mono-fiber strong force instrument and obtained, and folder is away from for 10mm, and rate of extension is 10mm/min, and electric rate passes through general-purpose
Table is measured.
Embodiment 1
Graphene/PNIPAM composite fibre process is prepared by 98/2 spinning solution of GO/PNIPAM mass ratioes such as
Under：
（1）2g graphene oxides are dissolved in 96g water, ultrasonic disperse 4h, obtain finely dispersed graphene oxide solution, plus
Enter 0.004g 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, activation 60min；Graphite oxide after activation
The 4g 1wt% PNIPAM aqueous solution is added in alkene solution, 24h is reacted, obtains composite spinning liquid；
（2）Will（1）The composite spinning liquid ultrasound 30min of gained, then with 15mL/h extruded velocity, is squeezed by aperture spinneret
After going out, 60s is stopped into 20 DEG C of acetic acid coagulating baths；Then hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, obtained
Graphene oxide composite fibre；
（3）By step（2）The graphene oxide composite fibre of gained is dried, and is placed in 90 DEG C of reduction 5min in reducing agent hydroiodic acid,
Drying is washed, graphene composite fibre is just can obtain.
Fig. 1 is graphene composite fibre heavy burden 5g counterweights manufactured in the present embodiment macroscopical digital photograph of 10 days.Fig. 2 is this
The microscope photograph of graphene composite fibre prepared by embodiment.It can be seen that the graphene fiber prepared by the present embodiment has
Good pliability.Its fracture strength of graphene composite fibre prepared by this embodiment is 2.3cN/tex, extension at break
20%, electrical conductivity is 9.2S/cm, as shown in table 1.
Embodiment 2
Graphene/PNIPAM composite fibre process is prepared by 95/5 spinning solution of GO/PNIPAM mass ratioes such as
Under：
（1）1.8g graphene oxides are dissolved in 95g water, ultrasonic disperse 4h obtains finely dispersed graphene oxide solution,
Add 0.003g 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, activation 60min；Oxidation stone after activation
The 5g 1.9wt% PNIPAM aqueous solution is added in black alkene solution, 24h is reacted, obtains composite spinning liquid；
（2）Will（1）The composite spinning liquid ultrasound 30min of gained, then with 15mL/h extruded velocity, is squeezed by aperture spinneret
After going out, 60s is stopped into 20 DEG C of acetic acid coagulating baths.Then hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, obtained
Graphene oxide composite fibre；
（3）By step（2）The graphene oxide composite fibre of gained is dried, and is placed in 90 DEG C of reduction 5min in reducing agent hydroiodic acid,
Drying is washed, graphene composite fibre is just can obtain.
Its fracture strength of graphene composite fibre prepared by the present embodiment is 4.5cN/tex, extension at break 22%, conductance
Rate is 11.6S/cm, as shown in table 1.
Embodiment 3
Graphene/PNIPAM composite fibre process is prepared by 92/8 spinning solution of GO/PNIPAM mass ratioes such as
Under：
（1）1.6g graphene oxides are dissolved in 90g water, ultrasonic disperse 4h obtains finely dispersed graphene oxide solution,
Add 0.002g 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, activation 60min；Oxidation stone after activation
The 10g 1.4wt% PNIPAM aqueous solution is added in black alkene solution, 24h is reacted, obtains composite spinning liquid；
（2）Will（1）The composite spinning liquid ultrasound 30min of gained, then with 15mL/h extruded velocity, is squeezed by aperture spinneret
After going out, 60s is stopped into 20 DEG C of acetic acid coagulating baths.Then hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, obtained
Graphene oxide composite fibre；
（3）By step（2）The graphene oxide composite fibre of gained is dried, and is placed in 90 DEG C of reduction 5min in reducing agent hydroiodic acid,
Drying is washed, graphene composite fibre is just can obtain.
Its fracture strength of graphene composite fibre prepared by the present embodiment is 8.5cN/tex, extension at break 14%, conductance
Rate is 14.2S/cm, as shown in table 1.
Embodiment 4
Graphene/PNIPAM composite fibre process is prepared by 90/10 spinning solution of GO/PNIPAM mass ratioes such as
Under：
（1）1.5g graphene oxides are dissolved in 90g water, ultrasonic disperse 4h obtains finely dispersed graphene oxide solution,
Add 0.002g 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, activation 60min；Oxidation stone after activation
The 10g 1.7wt% PNIPAM aqueous solution is added in black alkene solution, 24h is reacted, obtains composite spinning liquid；
（2）Will（1）The composite spinning liquid ultrasound 30min of gained, then with 15mL/h extruded velocity, is squeezed by aperture spinneret
After going out, 60s is stopped into 20 DEG C of acetic acid coagulating baths.Then hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, obtained
Graphene oxide composite fibre；
（3）By step（2）The graphene oxide composite fibre of gained is dried, and is placed in 90 DEG C of reduction 5min in reducing agent hydroiodic acid,
Drying is washed, graphene composite fibre is just can obtain.
Its fracture strength of graphene composite fibre prepared by this embodiment is 3.7cN/tex, extension at break 13%, electricity
Conductance is 14.6S/cm, as shown in table 1.
Embodiment 5
Graphene/PNIPAM composite fibre process is prepared by 90/10 spinning solution of GO/PNIPAM mass ratioes such as
Under：
（1）1.5g graphene oxides are dissolved in 90g water, ultrasonic disperse 4h obtains finely dispersed graphene oxide solution,
Add 0.002g 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, activation 60min；Oxidation stone after activation
The 10g 1.7wt% PNIPAM aqueous solution is added in black alkene solution, 24h is reacted, obtains composite spinning liquid；
（2）Will（1）The composite spinning liquid ultrasound 30min of gained, then with 15mL/h extruded velocity, is squeezed by aperture spinneret
After going out, 60s is stopped into 20 DEG C of acetic acid coagulating baths.Then hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, obtained
Graphene oxide composite fibre；
（3）By step（2）The graphene oxide composite fibre of gained is dried, and is placed in 90 DEG C of reduction in reducing agent hydroiodic acid
480min, washs drying, just can obtain graphene composite fibre.
Its fracture strength of graphene composite fibre prepared by this embodiment is 1.6cN/tex, extension at break 12%, electricity
Conductance is 22.0S/cm, as shown in table 1.
Reference examples
Graphene fiber preparation process without polymer is as follows：
（1）2g graphene oxides are dissolved in 100g water, ultrasonic disperse 4h obtains finely dispersed graphene oxide solution,
Then with 15mL/h extruded velocity, after being extruded by aperture spinneret, 60s is stopped into 20 DEG C of acetic acid coagulating baths.Then
Hygrometric state fiber is drawn into coagulating bath, after being dried through infrared lamp, graphene oxide composite fibre is obtained；
（2）The graphene oxide composite fibre of gained is dried, 90 DEG C of reduction 5min in reducing agent hydroiodic acid are placed in, washing is dry
It is dry, it just can obtain graphene composite fibre.
Fig. 3 is graphene fiber heavy burden 5g counterweight macroscopical digital photographs of 10 days prepared by this reference examples.This reference examples institute
Its fracture strength of the graphene composite fibre of preparation is 5.8cN/tex, and extension at break 14%, electrical conductivity is 5.3S/cm, such as the institute of table 1
Show.
With the diameter and data of mechanical of the graphene composite fibre of reference examples in the embodiment 1-5 of table 1.
Embodiment of above is merely to illustrate the present invention, and not limitation of the present invention, about the ordinary skill of technical field
Personnel, without departing from the spirit and scope of the present invention, can also make a variety of changes and modification, therefore all equivalent
Technical scheme fall within scope of the invention, scope of patent protection of the invention should be defined by the claims.
Claims (8)
1. a kind of amine based polymer composite graphite alkene height leads fiber, it is characterised in that：The fiber is that polymer graphite is modified alkene
Composite fibre, its fracture strength is more than 1.6cN/tex, and conductance is more than 9.2S/cm.
2. a kind of amine based polymer composite graphite alkene height leads the preparation method of fiber, it is characterised in that the preparation method includes
Following steps：
1）By the graphene oxide of 1 parts by weight, in the solvent for being added to 10~100 parts by weight, it is ultrasonically treated after obtain scattered equal
Even graphene oxide solution；
2）In above-mentioned steps 1）0.001~0.01 weight is added in the obtained finely dispersed graphene oxide solution of graphene oxide
The activator of part is measured, 10~120min, the graphene oxide solution after being activated is activated；
3）In above-mentioned steps 2）In the amino-containeds of 0.01~0.2 parts by weight is added in graphene oxide solution after obtained activation
Polymer, react 6~48h, obtain graphene oxide complex solution；
4）By above-mentioned steps 3）After the ultrasonically treated 5~60min of graphene oxide complex solution of gained, with 1~30mL/h's
Extruded velocity, after being extruded by aperture spinneret, into coagulating bath, stops 10~100s, so in 10~60 DEG C of coagulating bath
Dried afterwards with infrared lamp, obtain graphene oxide composite fibre；
5）By above-mentioned steps 4）The graphene oxide composite fibre of gained is dried, be placed in reducing agent 50~90 DEG C of reduction 5~
480min, washs drying, just can obtain graphene composite fibre.
3. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
State step 1）In solvent include water, N,N-dimethylformamide, 1-METHYLPYRROLIDONE, dimethyl sulfoxide in it is a kind of or many
Plant according to any proportioning mixing composition.
4. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
State step 2）In activator to include 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides, dicyclohexyl carbon two sub-
It is one or more kinds of according to any proportioning mixing composition in amine, BTA base diethyl phosphate.
5. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
State step 3）In amino-contained polymer be polyacrylamide, polycaprolactam, poly- N, N '-N-isopropylacrylamide, gather oneself
One kind in two acyl hexamethylene diamines, polydecamethylene adipamide, polyaniline, polythiophene, polypyrrole, chitosan, fibroin albumen.
6. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
State step 4）In coagulating bath include acetic acid, ethyl acetate, butyl acetate, methanol, ethanol, glycerine, acetone in one kind or
Person is a variety of according to any proportioning mixing composition.
7. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
State step 5）In reducing agent include sodium hydrogensulfite, hydroiodic acid, glucose, hydrazine hydrate, sodium borohydride, vitamin C in extremely
Few one kind.
8. amine based polymer composite graphite alkene height according to claim 2 leads the preparation method of fiber, it is characterised in that：Institute
The graphene oxide stated be graphite by pre-oxidation, peel off, oxidation, filtering, washing, dry after obtained graphite oxide
Alkene, is at least one of graphene oxide, carboxylated graphene oxide, sulfonic group graphene oxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109167024A (en) * | 2018-08-03 | 2019-01-08 | 常州大学 | The graphene oxide and preparation method thereof that more carbonyls for electrode material of lithium battery are modified |
| CN109267181A (en) * | 2018-09-26 | 2019-01-25 | 嘉兴学院 | A kind of preparation process with hollow structure graphene fiber |
| CN110158193A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | The preparation method of high molecular material based on modified graphene |
| WO2019211813A1 (en) * | 2018-05-03 | 2019-11-07 | Qi Diagnostics Limited | Chemical sensing device |
| CN111826946A (en) * | 2020-06-09 | 2020-10-27 | 江苏烨天羊绒科技有限公司 | Production method of wool and graphene blended yarn and fabric |
| CN113005565A (en) * | 2021-04-26 | 2021-06-22 | 南京工业大学 | Preparation method of high-strength bio-based composite fiber and composite fiber |
| CN114775090A (en) * | 2022-05-17 | 2022-07-22 | 凯盛家纺股份有限公司 | Preparation method of graphene modified anti-static fabric |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110158193A (en) * | 2018-04-12 | 2019-08-23 | 济南开发区星火科学技术研究院 | The preparation method of high molecular material based on modified graphene |
| WO2019211813A1 (en) * | 2018-05-03 | 2019-11-07 | Qi Diagnostics Limited | Chemical sensing device |
| CN109167024A (en) * | 2018-08-03 | 2019-01-08 | 常州大学 | The graphene oxide and preparation method thereof that more carbonyls for electrode material of lithium battery are modified |
| CN109267181A (en) * | 2018-09-26 | 2019-01-25 | 嘉兴学院 | A kind of preparation process with hollow structure graphene fiber |
| CN109267181B (en) * | 2018-09-26 | 2022-07-26 | 嘉兴学院 | Preparation process of graphene fiber with hollow structure |
| CN111826946A (en) * | 2020-06-09 | 2020-10-27 | 江苏烨天羊绒科技有限公司 | Production method of wool and graphene blended yarn and fabric |
| CN113005565A (en) * | 2021-04-26 | 2021-06-22 | 南京工业大学 | Preparation method of high-strength bio-based composite fiber and composite fiber |
| CN113005565B (en) * | 2021-04-26 | 2022-05-13 | 南京工业大学 | Preparation method of high-strength bio-based composite fiber and composite fiber |
| CN114775090A (en) * | 2022-05-17 | 2022-07-22 | 凯盛家纺股份有限公司 | Preparation method of graphene modified anti-static fabric |
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Application publication date: 20170808 |