CN102586916B - Preparation method for composite fiber of hyperbranched polymer grafted graphene - Google Patents
Preparation method for composite fiber of hyperbranched polymer grafted graphene Download PDFInfo
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- CN102586916B CN102586916B CN 201210014843 CN201210014843A CN102586916B CN 102586916 B CN102586916 B CN 102586916B CN 201210014843 CN201210014843 CN 201210014843 CN 201210014843 A CN201210014843 A CN 201210014843A CN 102586916 B CN102586916 B CN 102586916B
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Abstract
The invention discloses a preparation method for composite fiber of hyperbranched polymer grafted graphene. The preparation method comprises the following steps: adding 1 part by weight of graphene oxide, 50-2000 parts by weight of solvent and 1-100 parts by weight of hyperbranched polymer in a reactor, feeding nitrogen, heating, reaction, performing centrifugation, washing and drying to obtain the nanometer composite material of the hyperbranched polymer grafted graphene; dispersing the composite material of the hyperbranched polymer grafted graphene into solvent to obtain 1-50wt% of spinning slurry; causing the spinning slurry to pass through a spinning nozzle of which the diameter is 5-5000mu m at the extrusion speed of 1-100ml; staying for 1-3600s in solidification liquid at 5-30DEG Cfor solidifying and forming silk; and washing and drying in vacuum to obtain the composite fiber of the hyperbranched polymer grafted graphene. The spinning technology is simple and is operated at room temperature, and the process is environmentally friendly because of omitting a strong-corrosion reagent. The obtained fiber has excellent mechanical property and good toughness and can be applied to various fields of static electricity resistance, corrosion resistance and the like.
Description
Technical field
The present invention relates to a kind of composite fibre preparation method of grafted by super branched polymer Graphene.
Background technology
Graphene be one deck by carbon atom with sp
2The Two-dimensional Carbon atomic layer that hydridization is formed by connecting, its thickness only has 0.34 nm, is the thinnest two-dimensional nano material of finding at present.Find that after deliberation Graphene has superhigh intensity, great specific area, the speciality of the multiple excellences such as high thermal conductivity and carrier mobility, make it at transistor, ultracapacitor, permselectivity membrane, the numerous areas such as reinforcing material are with a wide range of applications.But Graphene is difficult to dissolving or disperses in common solvent, thereby has limited the further investigation of its structural behaviour and industrial extensive use.Research finds that chemical modification is the effective ways of preparation solubilized Graphene.Under the strong oxidizer effects such as the concentrated sulfuric acid, potassium persulfate, phosphorus pentoxide, potassium permanganate, hydrogen peroxide, through ultrasonic dispersion, can obtain graphene oxide (V. C. Tung such as native graphite, et al. Nat. Nanotechnol., 2009,4,25 – 29).
Graphene oxide can be dispersed in water and the N-methyl 2-Pyrrolidone isopolarity organic solvent preferably.Carry out functionalization and reduction take graphene oxide as raw material, can make the functionalization graphene with certain dispersiveness.At present preparation Graphene and composite thereof have become the study hotspot of material science, however most of research concentrate on the two-dimentional Graphene paper of preparation, prepare macroscopical Graphene composite fibre from graphene oxide and also fail to realize.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of composite fibre preparation method of grafted by super branched polymer Graphene is provided.
The composite fibre preparation method's of grafted by super branched polymer Graphene step is as follows:
1) in reactor, adds the graphene oxide of 1 weight portion, the solvent of 50-2000 weight portion, the dissaving polymer of 1-100 weight portion, logical nitrogen, be heated to 140-220 ℃, reaction 2-50 h, through centrifugal, washing, drying, obtain the grafted by super branched polymer graphene nanocomposite material, the quality percentage composition of dissaving polymer is 10-80%;
2) the grafted by super branched polymer graphene nanocomposite material is dispersed in the solvent, makes the spinning slurry that the quality percentage composition is 1-50%;
3) with spinning slurry take the extruded velocity of 1-100 mL/h by the spinning nozzle of diameter as 5-5000 μ m, in 5-30 ℃ solidification liquid, stop 1-3600s and be frozen into silk, washing, 40-80 degree centigrade of vacuumize 24 hours obtains the composite fibre of grafted by super branched polymer Graphene.
The solvent of described step 1) is selected from METHYLPYRROLIDONE, DMF, DMA, methyl-sulfoxide, sulfolane, perhaps their mixture.
Described step 2) dissaving polymer is selected from hyperbranched polyglycidyl ether, hyper-branched polyester, ultrabranching polyamide or their mixture.
Described step 2) solvent is selected from water, methyl alcohol, ethanol, ethylene glycol, diethylene glycol (DEG), METHYLPYRROLIDONE, DMF, DMA, methyl-sulfoxide, perhaps their mixture.
The coagulating agent of described step 3) is selected from the methyl alcohol of the aqueous solution, NaOH or KOH of NaOH or KOH or ethanolic solution, ether, ethyl acetate, acetone, benzinum, perhaps their mixture.
The diameter of the composite fibre of described grafted by super branched polymer Graphene is 5-5000 μ m.
Spinning technique of the present invention is simple, ambient operation, and without severe corrosive reagent, the process environmental protection, the gained fibrous mechanical property is excellent, and preferably toughness is arranged, and can be applicable to antistatic, a plurality of fields such as anticorrosive.
Description of drawings
Fig. 1 is that the composite fibre of hyperbranched polyglycidyl ether graft grapheme is wound on the digital camera photo on the polytetrafluoroethylene (PTFE) roller bearing, and fibre length reaches several meters;
Fig. 2 is the stress strain curve of the composite fibre of hyperbranched polyglycidyl ether graft grapheme.
The specific embodiment
Grafted by super branched polymer Graphene composite fibre preparation method's step is as follows:
1) in reactor, adds the graphene oxide of 1 weight portion, the solvent of 50-2000 weight portion, the dissaving polymer of 1-100 weight portion, logical nitrogen, be heated to 140-220 ℃, reaction 2-50 h, through centrifugal, washing, drying, obtain the grafted by super branched polymer graphene nanocomposite material, the quality percentage composition of dissaving polymer is 10-80%;
2) the grafted by super branched polymer graphene nanocomposite material is dispersed in the solvent, makes the spinning slurry that the quality percentage composition is 1-50%;
3) with spinning slurry take the extruded velocity of 1-100 mL/h by the spinning nozzle of diameter as 5-5000 μ m, in 5-30 ℃ solidification liquid, stop 1-3600s and be frozen into silk, washing, 40-80 degree centigrade of vacuumize 24 hours obtains the composite fibre of grafted by super branched polymer Graphene.
The solvent of described step 1) is selected from METHYLPYRROLIDONE, DMF, DMA, methyl-sulfoxide, sulfolane, perhaps their mixture.
Described step 2) dissaving polymer is selected from hyperbranched polyglycidyl ether, hyper-branched polyester, ultrabranching polyamide or their mixture.
Described step 2) solvent is selected from water, methyl alcohol, ethanol, ethylene glycol, diethylene glycol (DEG), METHYLPYRROLIDONE, DMF, DMA, methyl-sulfoxide, perhaps their mixture.
The coagulating agent of described step 3) is selected from the methyl alcohol of the aqueous solution, NaOH or KOH of NaOH or KOH or ethanolic solution, ether, ethyl acetate, acetone, benzinum, perhaps their mixture.
The diameter of the composite fibre of described grafted by super branched polymer Graphene is 5-5000 μ m.
Below by embodiment the present invention is specifically described; present embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; those skilled in the art's content according to the present invention is made some nonessential change and adjustment, all belongs to protection scope of the present invention.
Embodiment 1:
1) in reaction bulb, adds the 20mg graphene oxide, the 1g METHYLPYRROLIDONE, 2g hyperbranched polyglycidyl ether, logical nitrogen, be heated to 160 ℃, react 16 h, through centrifugal, N, the dinethylformamide washing, vacuumize obtains hyperbranched polyglycidyl ether graft grapheme nano composite material product, and wherein the weight content of hyperbranched polyglycidyl ether is 65%;
2) Graphene with 100 mg hyperbranched polyglycidyl ether grafting is incorporated in 0.1 mL DMF, makes the quality percentage composition and be 50% spinning slurry;
3) with the Graphene spinning solution colloidal sol of hyperbranched polyglycidyl ether grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, in 5 ℃ ethyl acetate, stop 50 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 40 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% hyperbranched polyglycidyl ether graft grapheme.
Embodiment 2:
1) in reaction bulb, adds the 20mg graphene oxide, 0.5g METHYLPYRROLIDONE, 20 mg hyperbranched polyglycidyl ethers, logical nitrogen, be heated to 140 ℃, reaction 24h, through centrifugal, N, the dinethylformamide washing, vacuumize obtains hyperbranched polyglycidyl ether graft grapheme nano composite material product, and wherein the weight content of hyperbranched polyglycidyl ether is 10%;
2) Graphene with 100 mg hyperbranched polyglycidyl ether grafting is incorporated in 0.9 mL water, makes the quality percentage composition and be 1% spinning slurry;
3) with the Graphene spinning solution colloidal sol of hyperbranched polyglycidyl ether grafting, take the extruded velocity of 100 mL/h by the spinning capillary of diameter as 5 μ m, in 30 ℃ KOH methanol solution, stop 5 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5 μ m, fracture strength after the 40 degree vacuumizes in 24 hours and be 100MPa, elongation at break and be the composite fibre of 10% hyperbranched polyglycidyl ether graft grapheme.
Embodiment 3:
1) in reaction bulb, adds the 20mg graphene oxide, the 40g sulfolane, 100mg hyper-branched polyester, logical nitrogen, be heated to 220 ℃, reaction 2h, through centrifugal, N, the dinethylformamide washing, vacuumize obtains hyper-branched polyester graft grapheme nano composite material product, and wherein the weight content of hyper-branched polyester is 30%;
2) Graphene with 100 mg hyper-branched polyester grafting is incorporated in 0.4 mL methyl alcohol, makes the quality percentage composition and be 20% spinning slurry;
3) with the Graphene spinning solution colloidal sol of hyper-branched polyester grafting, take the extruded velocity of 10 mL/h by the spinning capillary of diameter as 100 μ m, in 20 ℃ ether, stop 3600 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 100 μ m, fracture strength after the 60 degree vacuumizes in 24 hours and be 50MPa, elongation at break and be the composite fibre of 15% hyperbranched bunching ester graft grapheme.
Embodiment 4:
1) in reaction bulb, adds the 20mg graphene oxide, the 10g DMF, the 200mg hyper-branched polyester, logical nitrogen, be heated to 140 ℃, reaction 50h is through centrifugal, methanol wash, vacuumize obtains hyper-branched polyester graft grapheme nano composite material product, and wherein the weight content of hyper-branched polyester is 80%;
2) Graphene with 100 mg hyper-branched polyester grafting is incorporated in 0.1 mL ethanol, makes the quality percentage composition and be 50% spinning slurry;
3) with the Graphene spinning solution colloidal sol of hyper-branched polyester grafting, take the extruded velocity of 20mL/h by the spinning capillary of diameter as 50 μ m, in 5 ℃ acetone, stop 360 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 50 μ m, fracture strength after the 60 degree vacuumizes in 24 hours and be 80MPa, elongation at break and be the composite fibre of 8% hyper-branched polyester graft grapheme.
Embodiment 5:
1) in reaction bulb, adds the 20mg graphene oxide, the 10g DMA, the 200mg ultrabranching polyamide, logical nitrogen, be heated to 150 ℃, reaction 30h is through centrifugal, methanol wash, vacuumize obtains ultrabranching polyamide graft grapheme nano composite material product, and wherein the weight content of ultrabranching polyamide is 20%;
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.2 mL ethylene glycol, makes the quality percentage composition and be 33% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 800 μ m, in 20 ℃ the KOH aqueous solution, stop 1 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 800 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide ether graft grapheme.
Embodiment 6:
1) in reaction bulb, adds the 10mg graphene oxide, the 10g dimethyl sulfoxide (DMSO), the 200mg ultrabranching polyamide, logical nitrogen is heated to 150 ℃, reaction 30h, through centrifugal, methanol wash, vacuumize, obtain ultrabranching polyamide graft grapheme nano composite material product, wherein the weight content of ultrabranching polyamide is 40%.；
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.3 mL diethylene glycol (DEG), makes the quality percentage composition and be 25% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, in 20 ℃ the NaOH aqueous solution, stop 50 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide graft grapheme.
Embodiment 7:
1) in reaction bulb, adds the 10mg graphene oxide, the 10g dimethyl sulfoxide (DMSO), the 200mg ultrabranching polyamide, logical nitrogen is heated to 150 ℃, reaction 30h, through centrifugal, methanol wash, vacuumize, obtain ultrabranching polyamide graft grapheme nano composite material product, wherein the weight content of ultrabranching polyamide is 40%.；
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.3 mL METHYLPYRROLIDONE, makes the quality percentage composition and be 25% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, in 20 ℃ NaOH methanol solution, stop 50 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide graft grapheme.
Embodiment 8:
1) in reaction bulb, adds the 10mg graphene oxide, the 10g dimethyl sulfoxide (DMSO), the 200mg ultrabranching polyamide, logical nitrogen is heated to 150 ℃, reaction 30h, through centrifugal, methanol wash, vacuumize, obtain ultrabranching polyamide graft grapheme nano composite material product, wherein the weight content of ultrabranching polyamide is 40%.；
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.3 mL DMA, makes the quality percentage composition and be 25% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, in 20 ℃ NaOH ethanolic solution, stop 50 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide graft grapheme.
Embodiment 9:
1) in reaction bulb, adds the 10mg graphene oxide, the 10g dimethyl sulfoxide (DMSO), the 200mg ultrabranching polyamide, logical nitrogen is heated to 150 ℃, reaction 30h, through centrifugal, methanol wash, vacuumize, obtain ultrabranching polyamide graft grapheme nano composite material product, wherein the weight content of ultrabranching polyamide is 40%.；
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.3 mL methyl-sulfoxide, makes the quality percentage composition and be 25% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, in 5 ℃ benzinum, stop 50 s and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide graft grapheme.
Embodiment 10:
1) in reaction bulb, adds the 10mg graphene oxide, the 10g dimethyl sulfoxide (DMSO), the 200mg ultrabranching polyamide, logical nitrogen is heated to 150 ℃, reaction 30h, through centrifugal, methanol wash, vacuumize, obtain ultrabranching polyamide graft grapheme nano composite material product, wherein the weight content of ultrabranching polyamide is 40%.；
2) Graphene with 100 mg ultrabranching polyamide grafting is incorporated in 0.3 mL methyl-sulfoxide, makes the quality percentage composition and be 25% spinning slurry;
3) with the Graphene spinning solution colloidal sol of ultrabranching polyamide grafting, take the extruded velocity of 1 mL/h by the spinning capillary of diameter as 5000 μ m, stop 50 s in 20 ℃ KOH ethanolic solutions and be frozen into silk, the use wrapping head is collected, and obtains diameter 5000 μ m, fracture strength after the 80 degree vacuumizes in 24 hours and be 150MPa, elongation at break and be the composite fibre of 5% ultrabranching polyamide graft grapheme.
Claims (6)
1. the composite fibre preparation method of a grafted by super branched polymer Graphene is characterized in that its step is as follows:
1) in reactor, adds the graphene oxide of 1 weight portion, the solvent of 50-2000 weight portion, the dissaving polymer of 1-100 weight portion, logical nitrogen, be heated to 140-220 ℃, reaction 2-50 h, through centrifugal, washing, drying, obtain the grafted by super branched polymer graphene nanocomposite material, the quality percentage composition of dissaving polymer is 10-80%;
2) the grafted by super branched polymer graphene nanocomposite material is dispersed in the solvent, makes the spinning slurry that the quality percentage composition is 1-50%;
3) with spinning slurry take the extruded velocity of 1-100 mL/h by the spinning nozzle of diameter as 5-5000 μ m, in 5-30 ℃ solidification liquid, stop 1-3600s and be frozen into silk, washing, 40-80 degree centigrade of vacuumize 24 hours obtains the composite fibre of grafted by super branched polymer Graphene.
2. the composite fibre preparation method of a kind of grafted by super branched polymer Graphene as claimed in claim 1, it is characterized in that: the solvent of described step 1) is selected from METHYLPYRROLIDONE, N, dinethylformamide, N, N-dimethylacetylamide, methyl-sulfoxide, sulfolane, perhaps their mixture.
3. the composite fibre preparation method of a kind of grafted by super branched polymer Graphene as claimed in claim 1, it is characterized in that: the dissaving polymer of described step 1) is selected from hyperbranched polyglycidyl ether, hyper-branched polyester, ultrabranching polyamide or their mixture.
4. the composite fibre preparation method of a kind of grafted by super branched polymer Graphene as claimed in claim 1, it is characterized in that: solvent described step 2) is selected from water, methyl alcohol, ethanol, ethylene glycol, diethylene glycol (DEG), METHYLPYRROLIDONE, N, dinethylformamide, N, N-dimethylacetylamide, methyl-sulfoxide, perhaps their mixture.
5. the composite fibre preparation method of a kind of grafted by super branched polymer Graphene as claimed in claim 1, it is characterized in that: the solidification liquid of described step 3) is selected from the methyl alcohol of the aqueous solution, NaOH or KOH of NaOH or KOH or ethanolic solution, ether, ethyl acetate, acetone, benzinum, perhaps their mixture.
6. the composite fibre preparation method of a kind of grafted by super branched polymer Graphene as claimed in claim 1, it is characterized in that: the diameter of the composite fibre of described grafted by super branched polymer Graphene is 5-5000 μ m.
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| CN102926020A (en) * | 2012-11-14 | 2013-02-13 | 浙江大学 | Preparation method for polymer-grafted graphene laminated fiber with electrical conductivity and high-strength |
| CN103541043A (en) * | 2013-08-01 | 2014-01-29 | 华为技术有限公司 | Preparation method of electric graphene composite fiber |
| CN104112604A (en) * | 2014-05-29 | 2014-10-22 | 华为技术有限公司 | Graphene fiber-based supercapacitor and preparation method thereof |
| CN104232108B (en) * | 2014-09-10 | 2016-03-09 | 浙江碳谷上希材料科技有限公司 | A kind of preparation method of the pure inorganic substances compound membrane based on Graphene |
| CN104562276A (en) * | 2014-12-05 | 2015-04-29 | 淮安锦纶化纤有限公司 | Method for modifying chinlon 6 fibers and modified product |
| CN105200547B (en) * | 2015-10-19 | 2018-06-01 | 南通强生石墨烯科技有限公司 | A kind of preparation method of graphene-terylene nanometer composite fibre |
| CN105932202B (en) * | 2016-06-08 | 2018-09-07 | 广东工业大学 | A kind of porous hyper-branched polyester graphite oxide film and its preparation method and application |
| CN111978771B (en) * | 2019-05-21 | 2022-03-01 | 中车唐山机车车辆有限公司 | Modified graphene oxide, preparation method thereof, anticorrosive paint containing modified graphene oxide and preparation method |
| CN111235676B (en) * | 2020-03-19 | 2020-12-04 | 宁波市雪狼户外服饰有限公司 | Graphene-based pneumonia pathogen protection fabric and preparation method thereof |
| CN114351277B (en) * | 2021-12-15 | 2023-11-28 | 徐州丽君工艺品有限公司 | Graphene-quaternary ammonium salt antibacterial bed fabric and preparation method thereof |
| CN115182068B (en) * | 2022-08-11 | 2023-06-27 | 东莞信鸿工程塑料有限公司 | Polyamide fiber with high flame retardance and preparation method thereof |
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