CN113337908A - Graphene reinforced vinylon and preparation method thereof - Google Patents
Graphene reinforced vinylon and preparation method thereof Download PDFInfo
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- CN113337908A CN113337908A CN202110531675.9A CN202110531675A CN113337908A CN 113337908 A CN113337908 A CN 113337908A CN 202110531675 A CN202110531675 A CN 202110531675A CN 113337908 A CN113337908 A CN 113337908A
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- vinylon
- polyvinyl alcohol
- graphene
- spinning
- additive
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 84
- 229920002978 Vinylon Polymers 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000009987 spinning Methods 0.000 claims abstract description 81
- 239000000835 fiber Substances 0.000 claims abstract description 76
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 60
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 60
- 239000000243 solution Substances 0.000 claims abstract description 52
- 238000001914 filtration Methods 0.000 claims abstract description 51
- 238000000034 method Methods 0.000 claims abstract description 47
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000011550 stock solution Substances 0.000 claims abstract description 19
- 230000001112 coagulating effect Effects 0.000 claims abstract description 18
- 238000005520 cutting process Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000654 additive Substances 0.000 claims description 55
- 230000000996 additive effect Effects 0.000 claims description 54
- 239000002994 raw material Substances 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 229920000742 Cotton Polymers 0.000 description 10
- 238000004321 preservation Methods 0.000 description 7
- 239000004568 cement Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 108010073771 Soybean Proteins Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 235000019710 soybean protein Nutrition 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
Abstract
The invention discloses a graphene reinforced vinylon and a preparation method thereof, wherein the method comprises the following steps: step 1, washing polyvinyl alcohol with water; step 2, preparing polyvinyl alcohol solution; step 3, primary filtration; step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution; step 5, filtering again; step 6, spinning: fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber; step 7, stretching in a damp and hot mode; step 8, dry heat stretching; step 9, cooling; step 10, cutting off: cutting the cooled nascent fiber according to the required length requirement; step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing. The invention also provides the graphene reinforced vinylon prepared by the method. The graphene reinforced vinylon fiber prepared by the method has the characteristics of improved antibacterial performance, good anticorrosion effect, long product storage time and the like.
Description
Technical Field
The invention relates to a graphene vinylon composite fiber and a preparation method thereof, and particularly relates to a graphene reinforced vinylon and a preparation method thereof.
Background
Vinylon is a trade name for polyvinyl acetal fibers, also known as vinylon. The performance of the cotton is close to that of cotton, and the cotton is called synthetic cotton and is the variety with the highest hygroscopicity in the existing synthetic fibers.
Vinylon has good softness and heat retention, and has lower relative density than cotton, so that vinylon with the same weight as cotton can be woven into more clothes. Its thermal conductivity is low, so that its heat-insulating property is good. Vinylon is also better than cotton in abrasion resistance and strength, so vinylon can be blended with cotton in many aspects to save cotton. Vinylon is mainly used for making knitted fabrics such as outerwear, cotton jersey trousers, sports sweater and the like, and also can be used for canvas, fishing nets, surgical operation sutures, bicycle tire cords, filter materials and the like.
Polyvinyl formal fiber is not easy to ignite and is close to flame for melting and shrinking, a little flame is arranged at the top end during combustion, when the fibers are melted into colloidal flame and become bigger, the fibers have thick black smoke and emit bitter and fragrant smell, and black bead-shaped particles are left after combustion and can be crushed by fingers.
The vinylon cement pipe is also called vinylon pipe, vinylon cement cable protection pipe and vinylon cement cable pipe. The vinylon cement pipe is prepared by using vinylon fiber as basic material, plant fiber, high-strength high-friction vinylon and other material, high-grade cement as main material, and through rolling.
The vinylon is mainly classified into water-soluble vinylon and high-strength vinylon, and the high-strength high-modulus vinylon which resists hot water is applied to cement reinforcement; the water-soluble vinylon is applied to spinning or producing untwisted/low-twist fabrics; blending with protein to produce soybean protein fiber, etc.
Graphene is a novel two-dimensional nano carbon material, and has a wide application scene due to a special structure and material, the breaking strength of the graphene is 200 times higher than that of the best steel, and meanwhile, the graphene has good elasticity, and the stretching amplitude can reach 20% of the size of the graphene.
Disclosure of Invention
The invention aims to provide a graphene vinylon composite fiber and a preparation method thereof.
In order to achieve the above object, the present invention provides a method for preparing graphene reinforced vinylon, wherein the method comprises: step 1, washing polyvinyl alcohol: soaking, stirring and washing polyvinyl alcohol; step 2, preparing polyvinyl alcohol solution: uniformly mixing the washed polyvinyl alcohol with the graphene, the first additive and the second additive, dissolving and heating the mixture, and preparing the polyvinyl alcohol into a spinning solution; step 3, primary filtration: filtering the spinning solution; step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution; and 5, filtering again: filtering the defoamed spinning solution again; step 6, spinning: fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber; step 7, wet-heat stretching: stretching the as-spun fibers in a wet draw bath; step 8, dry heat stretching: drying the nascent fiber, and performing dry heat stretching in the drying process; and 9, cooling: cooling the dry-hot stretched nascent fiber at normal temperature; step 10, cutting off: cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon; step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
In the preparation method of the graphene reinforced vinylon, in the step 1, the polyvinyl alcohol is put into a washing machine for soaking, stirring and washing for 1-5 hours.
In the step 2, the washed polyvinyl alcohol, the graphene, the first additive and the second additive are put into a dissolving machine to be uniformly mixed, and are dissolved by a steam heating mode, so that the polyvinyl alcohol is prepared into the spinning solution.
In the step 3, the spinning solution is filtered by a gear pump of a dissolver, and the temperature is kept at 90-120 ℃ and the flow rate is kept at 280-350L/min during the filtering process.
In the preparation method of the graphene reinforced vinylon, in the step 4, the spinning solution is defoamed under the conditions of the heat preservation of 80-100 ℃ and the normal pressure of 0.01-0.3 MPa.
In the step 5, the defoamed spinning solution is filtered again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
In the above method for preparing graphene reinforced vinylon, in step 7, the nascent fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
In the step 8, when the surface temperature of the nascent fiber in the drying process reaches 210-230 ℃, dry-heat stretching is performed.
The invention also provides the graphene reinforced vinylon prepared by the method.
The graphene reinforced vinylon comprises the following raw materials in percentage by mass: 70-80% of polyvinyl alcohol, 1-5% of graphene, 5-12% of a first additive and 10-15% of a second additive; the first additive comprises sodium sulfate and/or magnesium sulfate; the second additive comprises any one or more of ethylene glycol, glycerol, and dimethyl sulfoxide.
The graphene reinforced vinylon and the preparation method thereof provided by the invention have the following advantages:
according to the invention, the graphene is added into the vinylon fiber, and the graphene has good ductility and strength and can enhance the tensile resistance of the fiber.
The graphene reinforced vinylon fiber prepared by the method has the characteristics of improved antibacterial performance, good anticorrosion effect, long product storage time and the like.
The graphene reinforced vinylon prepared by the method has the advantages of simple and easy operation process, low cost and high economic benefit, and is suitable for large-scale industrial production.
Detailed Description
The following further describes embodiments of the present invention.
The invention provides a preparation method of graphene reinforced vinylon, which comprises the following steps: step 1, washing polyvinyl alcohol: soaking, stirring and washing a polyvinyl alcohol (PVA) raw material; step 2, preparing polyvinyl alcohol solution: uniformly mixing the washed polyvinyl alcohol raw material with graphene, a first additive and a second additive, dissolving and heating, and preparing the polyvinyl alcohol raw material into a spinning solution; step 3, primary filtration: filtering the spinning solution; step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution; and 5, filtering again: filtering the defoamed spinning solution again; step 6, spinning: stirring all the obtained spinning stock solution to fully mix the spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber; step 7, wet-heat stretching: stretching the as-spun fibers in a wet draw bath; step 8, dry heat stretching: drying the nascent fiber, and performing dry heat stretching in the drying process; and 9, cooling: cooling the dry-hot stretched nascent fiber at normal temperature; step 10, cutting off: cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon; step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing at a certain temperature.
The equipment involved in the method is the existing equipment in the field.
Preferably, in step 1, the polyvinyl alcohol raw material is put into a washing machine for immersion, stirring and washing for 1 to 5 hours.
And 2, putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, and dissolving the polyvinyl alcohol raw material into spinning solution in a steam heating mode.
In the step 3, the spinning solution is filtered by a gear pump of a dissolving machine, and the temperature is kept at 90-120 ℃ and the flow rate is kept at 280-350L/min in the filtering process.
In step 4, the spinning solution is defoamed under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
In step 5, the defoamed spinning solution is filtered again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
In step 7, the as-spun fibers are drawn in a wet draw bath at a temperature of 80 ℃ to 98 ℃.
In step 8, the as-spun fiber in the drying process is subjected to dry heat drawing when the surface temperature thereof reaches 210 ℃ to 230 ℃.
The invention also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 70-80% of polyvinyl alcohol, 1-5% of graphene, 5-12% of a first additive and 10-15% of a second additive.
The first additive comprises sodium sulfate and/or magnesium sulfate; the second additive comprises any one or more of ethylene glycol, glycerol, and dimethyl sulfoxide.
The graphene-reinforced vinylon and the preparation method thereof provided by the invention are further described below with reference to the following examples.
Example 1
A method of preparing graphene reinforced vinylon, comprising:
step 1, washing polyvinyl alcohol: putting the polyvinyl alcohol raw material into a washing machine for soaking, stirring and washing for 1-5 hours.
Step 2, preparing polyvinyl alcohol solution: and putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, dissolving in a steam heating mode, and preparing the polyvinyl alcohol raw material into a spinning solution.
Step 3, primary filtration: filtering the spinning solution by a gear pump of a dissolving machine, and keeping the temperature at 90-120 ℃ and the flow rate at 280-350L/min in the filtering process.
Step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
And 5, filtering again: and filtering the defoamed spinning solution again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
Step 6, spinning: and fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber.
Step 7, wet-heat stretching: the as-spun fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
Step 8, dry heat stretching: drying the primary fiber, and performing dry heat stretching when the surface temperature of the primary fiber reaches 210-230 ℃ in the drying process of the primary fiber.
And 9, cooling: and cooling the dry-hot stretched nascent fiber at normal temperature.
Step 10, cutting off: and cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon.
Step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
The embodiment also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 80% of polyvinyl alcohol, 1% of graphene, 5% of a first additive and 14% of a second additive.
The first additive is sodium sulfate; the second additive comprises ethylene glycol.
Example 2
A method of preparing graphene reinforced vinylon, comprising:
step 1, washing polyvinyl alcohol: putting the polyvinyl alcohol raw material into a washing machine for soaking, stirring and washing for 1-5 hours.
Step 2, preparing polyvinyl alcohol solution: and putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, dissolving in a steam heating mode, and preparing the polyvinyl alcohol raw material into a spinning solution.
Step 3, primary filtration: filtering the spinning solution by a gear pump of a dissolving machine, and keeping the temperature at 90-120 ℃ and the flow rate at 280-350L/min in the filtering process.
Step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
And 5, filtering again: and filtering the defoamed spinning solution again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
Step 6, spinning: and fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber.
Step 7, wet-heat stretching: the as-spun fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
Step 8, dry heat stretching: drying the primary fiber, and performing dry heat stretching when the surface temperature of the primary fiber reaches 210-230 ℃ in the drying process of the primary fiber.
And 9, cooling: and cooling the dry-hot stretched nascent fiber at normal temperature.
Step 10, cutting off: and cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon.
Step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
The embodiment also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 76% of polyvinyl alcohol, 2% of graphene, 12% of a first additive and 10% of a second additive.
The first additive comprises magnesium sulfate; the second additive comprises glycerol.
Example 3
A method of preparing graphene reinforced vinylon, comprising:
step 1, washing polyvinyl alcohol: putting the polyvinyl alcohol raw material into a washing machine for soaking, stirring and washing for 1-5 hours.
Step 2, preparing polyvinyl alcohol solution: and putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, dissolving in a steam heating mode, and preparing the polyvinyl alcohol raw material into a spinning solution.
Step 3, primary filtration: filtering the spinning solution by a gear pump of a dissolving machine, and keeping the temperature at 90-120 ℃ and the flow rate at 280-350L/min in the filtering process.
Step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
And 5, filtering again: and filtering the defoamed spinning solution again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
Step 6, spinning: and fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber.
Step 7, wet-heat stretching: the as-spun fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
Step 8, dry heat stretching: drying the primary fiber, and performing dry heat stretching when the surface temperature of the primary fiber reaches 210-230 ℃ in the drying process of the primary fiber.
And 9, cooling: and cooling the dry-hot stretched nascent fiber at normal temperature.
Step 10, cutting off: and cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon.
Step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
The embodiment also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 74% of polyvinyl alcohol, 3% of graphene, 11% of a first additive and 12% of a second additive.
The first additive comprises sodium sulfate and magnesium sulfate; the second additive comprises dimethyl sulfoxide.
Example 4
A method of preparing graphene reinforced vinylon, comprising:
step 1, washing polyvinyl alcohol: putting the polyvinyl alcohol raw material into a washing machine for soaking, stirring and washing for 1-5 hours.
Step 2, preparing polyvinyl alcohol solution: and putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, dissolving in a steam heating mode, and preparing the polyvinyl alcohol raw material into a spinning solution.
Step 3, primary filtration: filtering the spinning solution by a gear pump of a dissolving machine, and keeping the temperature at 90-120 ℃ and the flow rate at 280-350L/min in the filtering process.
Step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
And 5, filtering again: and filtering the defoamed spinning solution again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
Step 6, spinning: and fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber.
Step 7, wet-heat stretching: the as-spun fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
Step 8, dry heat stretching: drying the primary fiber, and performing dry heat stretching when the surface temperature of the primary fiber reaches 210-230 ℃ in the drying process of the primary fiber.
And 9, cooling: and cooling the dry-hot stretched nascent fiber at normal temperature.
Step 10, cutting off: and cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon.
Step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
The embodiment also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 73% of polyvinyl alcohol, 4% of graphene, 10.5% of a first additive and 12.5% of a second additive.
The first additive comprises sodium sulfate; the second additive comprises ethylene glycol and glycerol.
Example 5
A method of preparing graphene reinforced vinylon, comprising:
step 1, washing polyvinyl alcohol: putting the polyvinyl alcohol raw material into a washing machine for soaking, stirring and washing for 1-5 hours.
Step 2, preparing polyvinyl alcohol solution: and putting the washed polyvinyl alcohol raw material, graphene, the first additive and the second additive into a dissolving machine for uniform mixing, dissolving in a steam heating mode, and preparing the polyvinyl alcohol raw material into a spinning solution.
Step 3, primary filtration: filtering the spinning solution by a gear pump of a dissolving machine, and keeping the temperature at 90-120 ℃ and the flow rate at 280-350L/min in the filtering process.
Step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution under the conditions of heat preservation of 80-100 ℃ and normal pressure of 0.01-0.3 MPa.
And 5, filtering again: and filtering the defoamed spinning solution again under the conditions of pressure of 0.01-0.3Mpa and flow rate of 25-175 ml/min.
Step 6, spinning: and fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber.
Step 7, wet-heat stretching: the as-spun fiber is drawn in a wet drawing bath at a temperature of 80 ℃ to 98 ℃.
Step 8, dry heat stretching: drying the primary fiber, and performing dry heat stretching when the surface temperature of the primary fiber reaches 210-230 ℃ in the drying process of the primary fiber.
And 9, cooling: and cooling the dry-hot stretched nascent fiber at normal temperature.
Step 10, cutting off: and cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon.
Step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
The embodiment also provides the graphene reinforced vinylon prepared by the method.
Preferably, the raw materials of the graphene reinforced vinylon comprise, by mass: 70% of polyvinyl alcohol, 5% of graphene, 10% of a first additive and 15% of a second additive.
The first additive comprises magnesium sulfate; the second additive comprises any of ethylene glycol, glycerol, dimethyl sulfoxide.
The graphene reinforced vinylon and the preparation method thereof provided by the invention are mainly characterized in that additives such as graphene and the like are added in the fiber preparation process and fully compounded, so that the tensile strength of vinylon fibers is further improved, the service life of vinylon fibers is prolonged, the fracture resistance is improved, and the like. The prepared graphene reinforced vinylon fiber also has the characteristics of improved antibacterial performance, good anticorrosion effect, long product storage time and the like.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (10)
1. A preparation method of graphene reinforced vinylon is characterized by comprising the following steps:
step 1, washing polyvinyl alcohol: soaking, stirring and washing polyvinyl alcohol;
step 2, preparing polyvinyl alcohol solution: uniformly mixing the washed polyvinyl alcohol with the graphene, the first additive and the second additive, dissolving and heating the mixture, and preparing the polyvinyl alcohol into a spinning solution;
step 3, primary filtration: filtering the spinning solution;
step 4, defoaming: removing bubbles generated in the primary filtration conveying process of the spinning solution;
and 5, filtering again: filtering the defoamed spinning solution again;
step 6, spinning: fully mixing the obtained spinning stock solution, injecting the spinning stock solution into a coagulating bath through a spinning metering pump, and dehydrating and coagulating to form nascent fiber;
step 7, wet-heat stretching: stretching the as-spun fibers in a wet draw bath;
step 8, dry heat stretching: drying the nascent fiber, and performing dry heat stretching in the drying process;
and 9, cooling: cooling the dry-hot stretched nascent fiber at normal temperature;
step 10, cutting off: cutting the cooled nascent fiber according to the required length requirement to obtain the graphene reinforced vinylon;
step 11, storage: and oiling the prepared graphene reinforced vinylon, and storing.
2. The method for preparing graphene reinforced vinylon according to claim 1, wherein in the step 1, the polyvinyl alcohol is put into a water washing machine for immersion, stirring and water washing for 1-5 hours.
3. The method of claim 1, wherein in the step 2, the polyvinyl alcohol after washing, the graphene, the first additive and the second additive are put into a dissolver to be uniformly mixed, and are dissolved by means of steam heating, so that the polyvinyl alcohol is prepared into the spinning solution.
4. The method for preparing graphene reinforced vinylon according to claim 1, wherein in the step 3, the spinning solution is filtered by a gear pump of a dissolver, and the temperature is kept at 90-120 ℃ and the flow rate is 280-350L/min during the filtering process.
5. The method of claim 1, wherein in step 4, the dope is defoamed at 80-100 ℃ under 0.01-0.3 MPa.
6. The method of claim 1, wherein in step 5, the defoamed dope is filtered again under a pressure of 0.01 to 0.3Mpa and a flow rate of 25ml/min to 175 ml/min.
7. The method of claim 1, wherein in step 7, the nascent fiber is drawn in a wet draw bath at a temperature of 80 ℃ to 98 ℃.
8. The method of claim 1, wherein in the step 8, the nascent fiber is subjected to dry heat stretching when the surface temperature of the nascent fiber reaches 210 ℃ to 230 ℃ during drying.
9. A graphene reinforced vinylon prepared by the method of any one of claims 1 to 8.
10. The graphene-reinforced vinylon according to claim 9, wherein the raw material of the graphene-reinforced vinylon comprises, by mass: 70-80% of polyvinyl alcohol, 1-5% of graphene, 5-12% of a first additive and 10-15% of a second additive; the first additive comprises sodium sulfate and/or magnesium sulfate; the second additive comprises any one or more of ethylene glycol, glycerol, and dimethyl sulfoxide.
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