CN111485300A - Manufacturing process and equipment of reduced graphene oxide fibers - Google Patents
Manufacturing process and equipment of reduced graphene oxide fibers Download PDFInfo
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- CN111485300A CN111485300A CN202010164244.9A CN202010164244A CN111485300A CN 111485300 A CN111485300 A CN 111485300A CN 202010164244 A CN202010164244 A CN 202010164244A CN 111485300 A CN111485300 A CN 111485300A
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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Abstract
A manufacturing process of reduced graphene oxide fibers comprises the following steps: preparing graphene oxide slurry; preparing a reducing agent solution, and inputting the reducing agent solution into a reaction tank; raising the temperature in the reaction tank; injecting the graphene oxide slurry into the reducing agent solution in the reaction tank by using an injector; starting the stirring paddle to make the reducing agent solution circularly flow; carrying out reduction reaction for 1-5 hours; and drying the reducing agent solution to prepare the reduced graphene oxide fiber. A manufacturing device of reduced graphene oxide fibers comprises a reaction tank, an inlet, an outlet, an inlet valve, an outlet valve, an electric heating wire, a stirring paddle and an injector. The method has the advantages of simple process, mild conditions, realization of continuous production to a great extent, high yield and easy industrialization.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a manufacturing process and equipment of reduced graphene oxide fibers.
Background
The graphene oxide fiber is a core process for preparing the graphene fiber; the graphene oxide has a natural graphite structure, and can improve the graphite structure in the reduction process to a greater extent, so that the graphene oxide has greater performance potential than high-temperature graphitization in the carbon fiber preparation process; how to prepare continuous and complete graphene oxide fibers is a prerequisite for solving the problem of graphene fiber preparation, and the main problem in the link is that graphene oxide contains a large amount of moisture and self gravity before drying, so that the continuity of graphene oxide is damaged, and the graphene oxide is difficult to form.
Disclosure of Invention
The invention aims to provide preparation equipment and a preparation process of reduced graphene oxide fibers, which have the advantages of simple process and mild conditions, can realize continuous production to a great extent, obtain higher yield and are easy to industrialize.
The technical scheme of the invention is as follows:
a manufacturing process of reduced graphene oxide fibers comprises the following steps:
step 1: preparing a graphene oxide solution from natural crystalline flake graphite powder by a hummers method, and centrifuging to remove water to obtain graphene oxide slurry with the solid content of 1% -5%.
And step 3: and electrifying the electric heating wire in the reaction tank to heat the reducing agent solution, so that the temperature of the reducing agent solution reaches 60-100 ℃.
And 4, injecting the graphene oxide slurry prepared in the step 1 into the reducing agent solution in the reaction tank at a constant speed by using an injector, wherein the injection speed is 5m L-10 ml/min.
And 5: starting a stirring paddle in the reaction tank, and slowly pushing the reducing agent solution in the reaction tank to circularly flow in the reaction tank.
Step 6: and (3) after finishing injecting the graphene oxide slurry, continuously carrying out reduction reaction for 1-5 hours, and keeping the reducing agent solution to circularly flow in the reaction tank.
And 7: and discharging the reducing agent solution in the reaction tank, and drying the reducing agent solution at 120-160 ℃ to obtain the reduced graphene oxide fiber.
Preferably, in the step 1, the mesh number of the natural crystalline flake graphite is preferably 100 to 5000 meshes, and most preferably 325 to 2000 meshes.
The manufacturing equipment for the reduced graphene oxide fibers comprises a reaction tank, wherein the reaction tank is a closed circulating pipeline and is provided with an inlet and an outlet, the inlet is provided with an inlet valve, and the outlet is provided with an outlet valve; the reaction tank is internally provided with an electric heating wire for heating and a stirring paddle for circulation; the needle nozzle of an injector penetrates through the shell of the reaction tank, extends into the cavity of the reaction tank and is fixed with the shell of the reaction tank.
The invention has the beneficial effects that:
1. the equipment structure is simple, the preparation period is short, and the structural integrity of the obtained reduced graphene oxide fiber is high;
2. the operation is safe, the toxicity of a strong reducing agent is avoided, and the reaction is mild and controllable;
3. the slurry can be subjected to surface reduction and rapid shaping in a liquid phase after injection, so that mutual adhesion is avoided, and the damage of the moisture weight of the graphene oxide to fibers is avoided by soaking in the liquid phase;
4. the graphene oxide fiber can be changed from hydrophilic to non-hydrophilic in the reduction process, a large amount of contained moisture is automatically removed, and the graphene oxide fiber shrinks after being drained in a liquid phase without being adhered to a base material, so that the shrinkage and fracture conditions are avoided;
5. the diameter size of the fiber can be adjusted by adjusting the injection speed and the solid content of the injected slurry, and the production is easy.
Drawings
Fig. 1 is a schematic structural diagram of a manufacturing apparatus for reducing graphene oxide fibers.
Detailed Description
Example 1:
a manufacturing process of reduced graphene oxide fibers comprises the following steps:
step 1: selecting 325-2000-mesh natural flake graphite, preparing a graphene oxide solution from natural flake graphite powder by a hummers method, and centrifuging to remove water to obtain graphene oxide slurry with the solid content of 1%.
And step 3: and electrifying the electric heating wire in the reaction tank to heat the reducing agent solution, so that the temperature of the reducing agent solution reaches 60 ℃.
And 4, injecting the graphene oxide slurry prepared in the step 1 into the reducing agent solution in the reaction tank at a constant speed by using an injector, wherein the injection speed is 10m L/min.
And 5: starting a stirring paddle in the reaction tank, and slowly pushing the reducing agent solution in the reaction tank to circularly flow in the reaction tank.
Step 6: and (3) after finishing injecting the graphene oxide slurry, continuously carrying out reduction reaction for 1 hour, and keeping the reducing agent solution to circularly flow in the reaction tank.
And 7: and discharging the reducing agent solution in the reaction tank, and drying the reducing agent solution at 120 ℃ to obtain the reduced graphene oxide fibers.
Example 2:
a manufacturing process of reduced graphene oxide fibers comprises the following steps:
step 1: selecting 325-2000-mesh natural flake graphite, preparing a graphene oxide solution from natural flake graphite powder by a hummers method, and centrifuging to remove water to obtain graphene oxide slurry with the solid content of 5%.
And step 3: and electrifying the electric heating wire in the reaction tank to heat the reducing agent solution so that the temperature of the reducing agent solution reaches 100 ℃.
And 4, injecting the graphene oxide slurry prepared in the step 1 into the reducing agent solution in the reaction tank at a constant speed by using an injector, wherein the injection speed is 5m L/min.
And 5: starting a stirring paddle in the reaction tank, and slowly pushing the reducing agent solution in the reaction tank to circularly flow in the reaction tank.
Step 6: and (4) after finishing injecting the graphene oxide slurry, continuously carrying out reduction reaction for 5 hours, and keeping the reducing agent solution to circularly flow in the reaction tank.
And 7: and discharging the reducing agent solution in the reaction tank, and drying the reducing agent solution at 160 ℃ to obtain the reduced graphene oxide fibers.
Example 3:
as shown in fig. 1, a manufacturing apparatus for reducing graphene oxide fibers includes a reaction tank 1, where the reaction tank 1 is a closed circulation pipeline, the reaction tank is provided with an inlet and an outlet, the inlet is provided with an inlet valve 5, and the outlet is provided with an outlet valve 6; the reaction tank 1 is internally provided with an electric heating wire 3 for heating and a stirring paddle 2 for circulation; the needle nozzle of an injector 4 penetrates through the shell of the reaction tank 1 to extend into the cavity of the reaction tank 1 and is fixed with the shell of the reaction tank 1.
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (3)
1. A manufacturing process of reduced graphene oxide fibers is characterized by comprising the following steps:
step 1: preparing a graphene oxide solution from natural crystalline flake graphite powder by a hummers method, and centrifuging to remove water to obtain graphene oxide slurry with the solid content of 1% -5%;
step 2, preparing a reducing agent solution with the concentration of 50 g/L-100 g/L by using ascorbic acid as a reducing agent, and inputting the reducing agent solution into a reaction tank;
and step 3: electrifying the electric heating wire in the reaction tank, and heating the reducing agent solution to enable the temperature of the reducing agent solution to reach 60-100 ℃;
step 4, injecting the graphene oxide slurry prepared in the step 1 into a reducing agent solution in a reaction tank at a constant speed by using an injector, wherein the injection speed is 5m L-10 ml/min;
and 5: starting a stirring paddle in the reaction tank, and slowly pushing the reducing agent solution in the reaction tank to circularly flow in the reaction tank;
step 6: after finishing injecting the graphene oxide slurry, continuously carrying out reduction reaction for 1-5 hours, and keeping the reducing agent solution to circularly flow in the reaction tank;
and 7: and discharging the reducing agent solution in the reaction tank, and drying the reducing agent solution at 120-160 ℃ to obtain the reduced graphene oxide fiber.
2. The process for preparing reduced graphene oxide fibers according to claim 1, wherein the process comprises the following steps: in the step 1, the mesh number of the natural crystalline flake graphite is preferably 100-5000 meshes, and most preferably 325-2000 meshes.
3. The utility model provides a preparation equipment of reduction oxidation graphite alkene fibre which characterized in that: the device comprises a reaction tank, wherein the reaction tank is a closed circulating pipeline and is provided with an inlet and an outlet, an inlet valve is arranged at the inlet, and an outlet valve is arranged at the outlet; the reaction tank is internally provided with an electric heating wire for heating and a stirring paddle for circulation; the needle nozzle of an injector penetrates through the shell of the reaction tank, extends into the cavity of the reaction tank and is fixed with the shell of the reaction tank.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115738950A (en) * | 2022-12-14 | 2023-03-07 | 中国科学技术大学 | Micro-fluidic-based graphene continuous preparation and assembly micro-system and application |
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