Preparation method of graphene oxide hollow fiber and graphene hollow fiber

A technology of graphene and graphene solution, which is applied in the manufacture of hollow filaments, fiber chemical characteristics, wet spinning, etc., can solve the problems of continuous production and post-processing, such as long time for impurity removal, and the inability to realize large batches, etc. And the effect of uniform internal structure, excellent mechanical properties, and simple operation process

CN103031618AActive Publication Date: 2013-04-10BEIJING TUNGHSU CARBON ADVANCED MATERIALS TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2013-04-10

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Abstract

The invention relates to a preparation method of a graphene oxide hollow fiber and a graphene hollow fiber, and belongs to the technical field of graphene oxide and graphene material preparation. The method comprises the following steps that an outer layer solution and an inner layer solution are respectively input into an outer layer and an inner layer of a coaxial needle head; the outer layer solution is injected into a receiving solution to form an aqueous graphene oxide hollow fiber, and then dried to form a graphene oxide hollow fiber; and the graphene oxide hollow fiber is reduced to a graphene hollow fiber. The outer layer solution is a 20-25mg.mL<-1> graphene oxide solution; the inner layer solution and the receiving solution are methanol solutions of KCL with a mass concentration greater than or equal to 3mol / L; the flow velocity of the inner layer solution is 0.6ml / min; and the flow velocity of the outer layer solution is greater than or equal to 0.1ml / s. According to the preparation method, the graphene oxide hollow fiber and the graphene hollow fiber can be prepared respectively in different steps of one method, the operation is easy and simple, aftertreatment and edulcoration are not required, the cost is low, and mass continuous production can be conducted.
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Description

technical field

[0001] The invention relates to a method for preparing graphene oxide and graphene hollow fibers. The method is a wet spinning method and belongs to the technical field of graphene oxide and graphene material preparation. Background technique

[0002] Single-layer sheet-like graphene (Graphene) composed of carbon atoms has high mechanical strength, elasticity, thermal conductivity and electron mobility (100,000cm 2 ·V -1 ·s -1 ). Graphene can be used in field-effect transistors, high-frequency devices, super microprocessors and single-molecule detectors. The three-dimensional structural materials composed of graphene as the basic unit, such as thin films and bulk materials, can be applied to the fields of functional materials such as controllable gas permeability films, anisotropic ion conductors, supercapacitors, lithium-ion batteries, and energy catalysis.

[0003] One of the main problems in the research and application of graphene is the effective ass...

Examples

Embodiment 1

[0035] (1) Prepare 20mg·mL by the improved Hummers method -1 The graphene oxide solution, concrete steps are as follows:

[0036] Mix 3g of graphite powder, 70ml of concentrated sulfuric acid (98% by mass with water) and 1.5ml of sodium nitrate, and stir evenly in a water bath at 0°C; then add 9g of potassium permanganate, and stir evenly; add after 0.5h 150ml of deionized water, and adjust the temperature of the water bath to 95°C for 15min; then add 500ml of deionized water and 15ml of H 2 o 2 (The mass percentage of water is 30%); the preliminary product is obtained, suction filtered, and the metal ions in the preliminary product are taken out with 250ml hydrochloric acid (36%-38% of the mass percentage of water), and then repeatedly washed with deionized water, Obtain a solid; ultrasonically disperse the solid with deionized water for 1 h to obtain a graphene oxide dispersion 1, then put the dispersion 1 into a centrifuge to remove the coagulated matter to obtain a dispe...

Embodiment 2

[0044] The 25 mg·mL prepared in step (1) of Example 1 -1 The graphene oxide solution was used as the outer layer solution, and the remaining steps were the same as step (2) of Example 1 to obtain a hydrated graphene oxide hollow fiber, which was dried naturally at 25° C. to obtain a graphene oxide hollow fiber.

[0045] Observation with a scanning electron microscope shows that the diameter of the hydrated graphene oxide hollow fiber is 700 μm; the hydrated graphene oxide hollow fiber presents a porous structure after freeze-drying; the surface structure of the graphene oxide hollow fiber is flat and the diameter is 470 μm.

[0046] Visual observation shows that the diameter of the graphene oxide hollow fiber shrinks to three-fifths of the diameter of the graphene oxide hollow fiber containing water.

[0047] Graphene oxide hollow fibers have excellent mechanical properties, good flexibility, and can be bent.

[0048] By using shimadzu AGS-X tensile tester to perform tensile ...

Embodiment 3

[0050] The graphene oxide hollow fiber prepared in Example 1 was placed in a tube furnace, and the graphene oxide hollow fiber was heat-treated in air at 400° C. for 1 h to obtain a graphene hollow fiber. The graphene hollow fiber was tensile tested using a shimadzu AGS-X tensile instrument, and its breaking strength was 173 MPa.

[0051] The graphene oxide hollow fiber prepared in Example 1 was put into hydroiodic acid, and kept at 80° C. for 8 hours to obtain a graphene hollow fiber. Using shimadzu AGS-X tensile instrument to carry out tensile test on graphene hollow fiber, it can be known that its breaking strength is 221MPa.