CN107653519A - A kind of preparation method of graphene fiber - Google Patents

A kind of preparation method of graphene fiber Download PDF

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Publication number
CN107653519A
CN107653519A CN201710992587.2A CN201710992587A CN107653519A CN 107653519 A CN107653519 A CN 107653519A CN 201710992587 A CN201710992587 A CN 201710992587A CN 107653519 A CN107653519 A CN 107653519A
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CN
China
Prior art keywords
solution
graphene
graphene fiber
preparation
graphene oxide
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CN201710992587.2A
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Chinese (zh)
Inventor
朱洋
邵蓉
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Nanjing Xuyurui Material Technology Co Ltd
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Nanjing Xuyurui Material Technology Co Ltd
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Priority to CN201710992587.2A priority Critical patent/CN107653519A/en
Publication of CN107653519A publication Critical patent/CN107653519A/en
Pending legal-status Critical Current

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Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments

Abstract

The invention discloses a kind of preparation method of graphene fiber, preparation process is:A takes partial oxidation of graphite alkene to be positioned over inside compound ion solution, finely dispersed afterwards to be stirred using ultrasonic disperse;B will add chloroacetic acid solution in the graphene oxide solution obtained in A, mixing time is maintained at 13 hours;The solution obtained in B is cooled to room temperature state by C, is carried out multistage filtering using filter membrane, is dried afterwards, obtains carboxylated graphene oxide;The material obtained in C is carried out ultrasonic disperse in N dimethyl formyl solution by D, carries out spinning and graphene fiber is made.Method is simple, is easy to industrialize, and graphene fiber conducts electricity very well, while has higher flexibility, there is huge application prospect in fields such as energy storage device, photovoltaic device, sensors;Be not in the excellent function of undesirable substance interference graphene fiber in whole preparation process, ensure that graphene fiber can effectively play its function.

Description

A kind of preparation method of graphene fiber
Technical field
The present invention relates to the preparation method technical field of graphene related substances material, specially a kind of graphene fiber Preparation method.
Background technology
Graphene is a kind of new material for the monolayer honeycomb shape structure being made up of carbon atom, is the structure of other dimension carbon materials Make basis.Graphene has many unique properties, such as high electron mobility, high thermal conductivity coefficient, good elasticity and rigidity. Therefore, graphene is assembled into functional structure such as fiber of macroscopic view etc., is the important channel for realizing graphene practical application.
Existing graphene fiber preparation method, it is excessively cumbersome, easily occur undesirable substance interference in whole preparation process The excellent function of graphene fiber, it is set effectively to play its function.Therefore, a kind of graphene fiber is herein proposed Novel processing step, solve the problems, such as mentioned above.
The content of the invention
It is an object of the invention to provide a kind of preparation method of graphene fiber, to solve to propose in above-mentioned background technology The problem of.
To achieve the above object, the present invention provides following technical scheme:A kind of preparation method of graphene fiber, the graphite The material and solution applied in the preparation process of alkene fiber includes:Graphene oxide, compound ion solution, chloroacetic acid solution, Filter membrane, N- dimethyl formyls, the preparation process of graphene fiber are:
A takes partial oxidation of graphite alkene to be positioned over inside compound ion solution, finely dispersed afterwards to be stirred using ultrasonic disperse Mix;
B will add chloroacetic acid solution in the graphene oxide solution obtained in A, and be stirred at 70-75 DEG C, and stir Mixing the time is maintained at 1-3 hours;
The solution obtained in B is cooled to room temperature state by C, and multistage filtering, the filter membrane diameter of bore model of filtering are carried out using filter membrane Enclose for 0.01-0.1mm, be dried afterwards, obtain carboxylated graphene oxide;
The material obtained in C is carried out ultrasonic disperse in N- dimethyl formyl solution by D, obtained solution, is carried out spinning and is made Graphene fiber.
Preferably, the ultrasonic disperse time span in the step A is 1-2.5 hours.
Preferably, the cooperation ratio in the step A between graphene oxide and compound ion solution is 0.3-0.5mg/ In ml, the step B, the mass ratio between graphene oxide solution and chloroacetic acid solution is 40-45.
Preferably, the rotating speed stirred in the step B is 100-150 revs/min.
Preferably, carboxylated graphene oxide and the mass volume ratio value of N- dimethyl formyl solution are in the step D 0.01-0.02mg/ml。
Compared with prior art, the beneficial effects of the invention are as follows:The preparation method of the graphene fiber, method is simple, easily In industrialization, graphene fiber conducts electricity very well, while has higher flexibility, in energy storage device, photovoltaic device, sensing There is huge application prospect in the fields such as device;Be not in the excellent work(of undesirable substance interference graphene fiber in whole preparation process Can, ensure that graphene fiber can effectively play its function.
Embodiment
It is clearly and completely described below in conjunction with the technical scheme in the embodiment of the present invention, it is clear that described reality It is only part of the embodiment of the present invention to apply example, rather than whole embodiments.It is general based on the embodiment in the present invention, this area The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected Scope.
, it is necessary to explanation in description of the invention, the orientation of instruction such as term " vertical ", " on ", " under ", " level " or Person's position relationship is for only for ease of the description present invention and simplifies description, rather than instruction either implies signified device or member Part must have specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.This Outside, " first ", " second ", " the 3rd ", " the 4th " are only used for describing purpose, and it is not intended that indicating or implying relatively important Property.In description of the invention, it is also necessary to explanation, unless otherwise clear and definite regulation and limitation, term " setting ", " installation ", " connected ", " connection ", it should be interpreted broadly, for example, it may be connecting or being fixedly connected or detachably connect Connect, or integrally connected, it can be mechanical connection or electrical connection, can be directly connected to or by middle matchmaker It is situated between and is connected, can is the connection of two element internals.For the ordinary skill in the art, can be as the case may be Understand the concrete meaning of above-mentioned term in the present invention.
The present invention provides a kind of technical scheme:A kind of preparation method of graphene fiber, the preparation of the graphene fiber The material and solution applied in journey includes:Graphene oxide, compound ion solution, chloroacetic acid solution, filter membrane, N- dimethyl methyls Acyl, the preparation process of graphene fiber are:
A takes partial oxidation of graphite alkene to be positioned over inside compound ion solution, finely dispersed afterwards to be stirred using ultrasonic disperse Mix;
B will add chloroacetic acid solution in the graphene oxide solution obtained in A, and be stirred at 70-75 DEG C, and stir Mixing the time is maintained at 1-3 hours;
The solution obtained in B is cooled to room temperature state by C, and multistage filtering, the filter membrane diameter of bore model of filtering are carried out using filter membrane Enclose for 0.01-0.1mm, be dried afterwards, obtain carboxylated graphene oxide;
The material obtained in C is carried out ultrasonic disperse in N- dimethyl formyl solution by D, obtained solution, is carried out spinning and is made Graphene fiber.
Preferably, the ultrasonic disperse time span in the step A is 1-2.5 hours.
Preferably, the cooperation ratio in the step A between graphene oxide and compound ion solution is 0.3-0.5mg/ In ml, the step B, the mass ratio between graphene oxide solution and chloroacetic acid solution is 40-45.
Preferably, the rotating speed stirred in the step B is 100-150 revs/min.
Preferably, carboxylated graphene oxide and the mass volume ratio value of N- dimethyl formyl solution are in the step D 0.01-0.02mg/ml。
The preparation method of the graphene fiber, method is simple, is easy to industrialize, and graphene fiber conducts electricity very well, simultaneously With higher flexibility, there is huge application prospect in fields such as energy storage device, photovoltaic device, sensors;It is whole to prepare During be not in undesirable substance interference graphene fiber excellent function, ensure graphene fiber can effectively play it Function.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (5)

  1. A kind of 1. preparation method of graphene fiber, it is characterised in that:The thing applied in the preparation process of the graphene fiber Matter and solution include:Graphene oxide, compound ion solution, chloroacetic acid solution, filter membrane, N- dimethyl formyls, graphene fiber Preparation process be:
    A takes partial oxidation of graphite alkene to be positioned over inside compound ion solution, finely dispersed afterwards to be stirred using ultrasonic disperse Mix;
    B will add chloroacetic acid solution in the graphene oxide solution obtained in A, and be stirred at 70-75 DEG C, and stir Mixing the time is maintained at 1-3 hours;
    The solution obtained in B is cooled to room temperature state by C, and multistage filtering, the filter membrane diameter of bore model of filtering are carried out using filter membrane Enclose for 0.01-0.1mm, be dried afterwards, obtain carboxylated graphene oxide;
    The material obtained in C is carried out ultrasonic disperse in N- dimethyl formyl solution by D, obtained solution, is carried out spinning and is made Graphene fiber.
  2. A kind of 2. preparation method of graphene fiber according to claim 1, it is characterised in that:It is super in the step A Sound jitter time length is 1-2.5 hours.
  3. A kind of 3. preparation method of graphene fiber according to claim 1, it is characterised in that:Aoxidized in the step A Cooperation ratio between graphene and compound ion solution is 0.3-0.5mg/ml, in the step B, graphene oxide solution and Mass ratio between chloroacetic acid solution is 40-45.
  4. A kind of 4. preparation method of graphene fiber according to claim 1, it is characterised in that:Stirred in the step B Rotating speed be 100-150 revs/min.
  5. A kind of 5. preparation method of graphene fiber according to claim 1, it is characterised in that:Carboxyl in the step D The mass volume ratio value for changing graphene oxide and N- dimethyl formyl solution is 0.01-0.02mg/ml.
CN201710992587.2A 2017-10-23 2017-10-23 A kind of preparation method of graphene fiber Pending CN107653519A (en)

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Application Number Priority Date Filing Date Title
CN201710992587.2A CN107653519A (en) 2017-10-23 2017-10-23 A kind of preparation method of graphene fiber

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977162A (en) * 2018-04-13 2018-12-11 太仓运通新材料科技有限公司 PA solvent-free thermal melten gel and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105887244A (en) * 2016-06-27 2016-08-24 苏州宇希新材料科技有限公司 Graphene fiber
CN106120024A (en) * 2016-06-27 2016-11-16 苏州宇希新材料科技有限公司 A kind of preparation method of graphene fiber
CN106149083A (en) * 2015-04-02 2016-11-23 恒天海龙股份有限公司 Functional graphene cellulose fiber prepared by melting method and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106149083A (en) * 2015-04-02 2016-11-23 恒天海龙股份有限公司 Functional graphene cellulose fiber prepared by melting method and preparation method thereof
CN105887244A (en) * 2016-06-27 2016-08-24 苏州宇希新材料科技有限公司 Graphene fiber
CN106120024A (en) * 2016-06-27 2016-11-16 苏州宇希新材料科技有限公司 A kind of preparation method of graphene fiber

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
伊势典夫等: "《高分子 胶体化学新论》", 30 June 2007, 西安:陕西科学技术出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977162A (en) * 2018-04-13 2018-12-11 太仓运通新材料科技有限公司 PA solvent-free thermal melten gel and preparation method thereof

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