Preparation method for graphene reinforced polymer porous sponge fiber

A porous sponge and polymer technology, applied in the direction of single-component synthetic polymer rayon, chemical post-treatment of synthetic polymer rayon, fiber treatment, etc., to achieve the effect of low density, large specific surface area, and easy large-scale production

Inactive Publication Date: 2014-02-26

QINGDAO UNIV

2 Cites 34 Cited by

AI-Extracted Technical Summary

Problems solved by technology

But so far, research on graphene-reinforced composite fibers (CN 103046151 A, CN 102828267 A, CN 102586951 A, CN 102926020 A, CN 102534837 A) is limited to the mixing of graphene solutions with other blendable polymers, Graphene-polymer composite fibe...

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Method used

The graphene-reinforced polymer porous sponge composite fiber prepared by the present invention, through the addition of graphene, has both realized the relatively large improvement of fiber aspect...

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Abstract

The invention provides a preparation method for graphene reinforced polymer porous sponge fiber. The preparation method is characterized in that: the graphene reinforced polymer porous sponge fiber is prepared by subjecting an oxidized graphene solution having a certain concentration to ultrasonic processing to obtain a uniformly dispersed oxidized graphene solution; dissolving a polymer in a solvent to obtain a polymer solution with a certain concentration; adding the dispersed graphene solution into the polymer solution under stirring to obtain a graphene-polymer blend spinning solution; spraying the graphene-polymer blend spinning solution through a spinning nozzle into a coagulating bath to form fiber by utilization of a wet-method spinning device; washing with water, reducing, and washing with water again; and quickly subjecting the wet fiber to freeze drying or supercritical drying to obtain the graphene reinforced polymer porous sponge fiber. The preparation method is simple in technology and low in cost, and is suitable for large-scale production. The fiber has advantages of high strength, good antistatic performance, good elasticity, small density, large specific surface area, and the like. The fiber can be used for preparing heat insulating fabrics in the weaving field, and can be used for water treatment in the environment protection field, and the like.

Application Domain

Artificial filaments from viscoseAlginate artificial filaments +5

Technology Topic

SolventCvd graphene +10

Examples

Experimental program(4)

Example Embodiment

[0021] The specific embodiment of the preparation method of a graphene-enhanced polymer porous sponge fiber of the present invention comprises the following steps:

[0022] (1) Under the condition of room temperature, a certain concentration of graphene oxide solution is ultrasonically treated in a 1-50 Hz ultrasonic bath for 0.5-1 h to obtain a uniformly dispersed graphene oxide solution. A certain amount of polymer is dissolved in the corresponding solvent to obtain a polymer solution with a certain concentration. The uniformly dispersed graphene oxide dispersion solution is added to the polymer solution, slowly added while stirring, and after complete addition, the stirring is continued for 4-8 hours to obtain a uniformly mixed graphene oxide-polymer blend spinning solution.

[0023] (2) The graphene oxide-polymer blended spinning solution is allowed to stand for deaeration for 8-12 hours, then transferred to the wet spinning equipment, and the spinning solution is sprayed into the coagulation using a spinneret with a diameter of 0.07-0.1 mm. It is solidified into fibers in a bath, and after washing with water, an intermediate product of wet graphene oxide-polymer blend fibers is obtained.

[0024] (3) Select a reducing agent with a mass concentration of 1-50%, weigh the wet graphene oxide-polymer blend fiber according to the ratio of the liquor ratio of 1:10-1:50, and reduce it at 30-95 °C For 0.5-2h, wet graphene-polymer blend fibers are obtained after washing with water. Freeze-drying or supercritical drying the wet graphene-polymer blend fibers to obtain graphene-polymer porous sponge fibers.

[0025] (4) The polymer used in the present invention is one or more of polyacrylonitrile, regenerated cellulose, sodium alginate and other polymers that can be wet-spun and can be blended with graphene oxide; The solvent and coagulation bath used are selected according to the traditional solvent and coagulation bath used in the preparation of polyacrylonitrile fibers, regenerated cellulose fibers and sodium alginate fibers; the reducing agents used are hydrazine, methylhydrazine, phenylhydrazine, NaOH , KOH, ammonia or hydroiodic acid, etc.

Example Embodiment

[0027] Example 1

[0028] (1) Under room temperature conditions, the graphene oxide solution with a mass concentration of 2.5% was ultrasonically treated in an ultrasonic bath at 1 Hz for 0.5 h to obtain a uniformly dispersed graphene oxide solution. Then a certain amount of regenerated cellulose pulp is impregnated, pressed, pulverized, aged, yellowed and dissolved to obtain a regenerated cellulose solution, wherein the solid content in the spinning solution: 6.81%, alkali content: 4.56%, viscosity: 41s, maturity: 8ml (10%NH4Cl), add the uniformly dispersed graphene oxide solution to the regenerated cellulose solution, the mass ratio of graphene in the mixed solution is 5%, slowly add it while stirring, and wait until it is completely added. Continue to stir for 4h to obtain a homogeneously mixed graphene oxide-regenerated cellulose blend spinning solution.

[0029] (2) The graphene oxide-regenerated cellulose blended spinning solution was left to stand for deaeration for 8 hours, transferred to a wet spinning equipment, and the spinning solution was sprayed into a coagulation bath using a spinneret with a diameter of 0.09 mm for coagulation. Fiber-forming, wherein the composition of the coagulation bath is: the concentration of sulfuric acid is 130g/L, the concentration of sodium sulfate is 330g/L, the concentration of zinc sulfate is 11.5g/L, and the temperature is 50°C. The product is a wet graphene oxide-regenerated cellulose blend fiber.

[0030] (3) Select a hydrazine hydrate reducing agent with a mass concentration of 50%, weigh the wet graphene oxide-regenerated cellulose blend fiber according to the ratio of the liquor ratio of 1:50, reduce it at 30 °C for 2 hours, and wash it with water to obtain Wet graphene-regenerated cellulose blend fibers. The wet graphene-regenerated cellulose blend fibers are frozen and formed at -80°C, and then freeze-dried to obtain graphene-regenerated cellulose porous sponge fibers.

[0031] (4) The graphene-regenerated cellulose porous sponge fiber obtained by this method has a fineness of 4.44dtex, a dry breaking strength of 2.9cN/dtex, and a mass specific resistance of 8.3×10 6 Ω·g/cm 2 , the density is 0.08g/cm 3.

Example Embodiment

[0032] Example 2

[0033] (1) Under room temperature conditions, the graphene oxide solution with a mass concentration of 3% was ultrasonically treated in an ultrasonic bath at 25 Hz for 0.8 h to obtain a uniformly dispersed graphene oxide solution. A certain amount of polyacrylonitrile is dissolved in a certain concentration of DMF solution to obtain a polyacrylonitrile solution. Add the uniformly dispersed graphene oxide solution into the polyacrylonitrile solution, wherein the content of graphene oxide in the mixed solution is 8%, slowly add while stirring, and continue to stir for 5 hours after complete addition to obtain uniformly mixed graphene oxide - Polyacrylonitrile blended spinning solution.

[0034] (2) The graphene oxide-polyacrylonitrile blended spinning solution was allowed to stand for deaeration for 9 hours, transferred to a wet spinning equipment, and the spinning solution was sprayed into a coagulation bath using a spinneret with a diameter of 0.08 mm to coagulate into a coagulation solution. Fiber, the coagulation bath is a mixed solution of water and N,N-dimethylacetamide (DMAc), and the fiber is washed with water after being formed to obtain an intermediate product of wet graphene oxide-polyacrylonitrile blend fiber.

[0035] (3) Methylhydrazine with a mass concentration of 8% was selected as the reducing agent, and the wet graphene oxide-polyacrylonitrile blend fiber was weighed according to the ratio of the liquor ratio of 1:20, and was reduced at 50 °C for 0.8 h. After washing with water, wet graphene-polyacrylonitrile blend fibers were obtained. The wet graphene-polyacrylonitrile blend fiber is freeze-dried or supercritically dried at -80°C to obtain the graphene-polyacrylonitrile porous sponge fiber.

[0036] (4) The graphene-polyacrylonitrile porous sponge fiber obtained by this method has a fineness of 4.44dtex, a dry breaking strength of 5.6cN/dtex, and a mass specific resistance of 1.2×10 6 Ω·g/cm 2 , the density is 0.08g/cm 3.

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PUM

Property	Measurement	Unit
Fineness	4.44	dtex
Dry breaking strength	2.9	cN/dtex
Mass specific resistance	8300000.0	g·Ω/cm²
tensile		MPa
Particle size		Pa
strength	10

Description & Claims & Application Information

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Preparation method for graphene reinforced polymer porous sponge fiber

A porous sponge and polymer technology, applied in the direction of single-component synthetic polymer rayon, chemical post-treatment of synthetic polymer rayon, fiber treatment, etc., to achieve the effect of low density, large specific surface area, and easy large-scale production

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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