CN110747580A - Preparation method of graphene heating fabric - Google Patents

Preparation method of graphene heating fabric Download PDF

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Publication number
CN110747580A
CN110747580A CN201911066302.8A CN201911066302A CN110747580A CN 110747580 A CN110747580 A CN 110747580A CN 201911066302 A CN201911066302 A CN 201911066302A CN 110747580 A CN110747580 A CN 110747580A
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temperature
graphene
gel
solution
solidified
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CN110747580B (en
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夏峰
夏耀忠
张哲志
程杰
冯超
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Bondwell Protection Polytron Technologies Inc
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Bondwell Protection Polytron Technologies Inc
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0015Electro-spinning characterised by the initial state of the material
    • D01D5/003Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/0007Electro-spinning
    • D01D5/0061Electro-spinning characterised by the electro-spinning apparatus
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00Heating or cooling textile fabrics

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dispersion Chemistry (AREA)
  • Artificial Filaments (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention belongs to the field of fabrics, and particularly relates to a preparation method of a graphene heating fabric, which comprises the following steps: step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution; step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed; step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns; step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric; and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric. The invention solves the problem of poor heat-insulating effect of the existing fabric, and the graphene fabric is utilized to form an electric heating system, so that a good heat-insulating effect is realized.

Description

Preparation method of graphene heating fabric
Technical Field
The invention belongs to the field of fabrics, and particularly relates to a preparation method of a graphene heating fabric.
Background
The fabric is a material for manufacturing the clothes, is one of three elements of the clothes, and not only can explain the style and the characteristics of the clothes, but also directly controls the expression effect of the clothes shape. In the field of clothing, various fabrics can be eight-door-five, which is different every day. However, in general, high-quality and high-grade fabrics have the characteristics of comfortable wearing, light weight, good visual effect, soft touch and the like. The warm-keeping effect of the warm-keeping fabric is considered, the warm-keeping effect is usually achieved through two aspects, the warm-keeping effect is achieved through natural animal fur with the good warm-keeping effect, the warm-keeping effect is achieved through thickening the fabric, and the fillers such as silk, feather or three-dimensional fiber are added to the inner layer of the clothes, so that air is stagnated in gaps of the clothes, the poor heat conduction of the air is utilized, the heat insulation effect is achieved, the body temperature is maintained or loss is reduced, and the purpose of keeping warm is achieved.
Although the two treatment modes belong to the conventional treatment mode, the customer acceptance is gradually reduced based on the problems of resource shortage, great reduction of comfort and the like. In the face of this problem, people are studying a novel fabric, which can generate heat by using an electric heating method to achieve a good warm-keeping effect.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a graphene heating fabric, which solves the problem of poor heat preservation effect of the existing fabric, and realizes good heat preservation effect by forming an electric heating system by using the graphene fabric.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of a graphene heating fabric comprises the following steps:
step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution;
step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed;
step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns;
step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric;
and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric.
The mass ratio of the graphene to the polypyrrole gel in the step 1 is 4:0.5-1, the adding amount of the distilled water is 300-450% of the mass of the graphene, the frequency of the ultrasonic is 40-80kHz, the temperature is 40-50 ℃, the temperature of the reduced pressure distillation is 120-150 ℃, the pressure is 70-80% of the atmospheric pressure, and the volume of the gel liquid is 20-30% of the solution before the reduced pressure distillation.
The concentration of the butyl rubber in the step 2 in the titanium tetrachloride is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the alumina is 150-300% of the mass of the butyl rubber, the temperature of the reduced pressure distillation is 150-170 ℃, and the pressure is 80-90% of the atmospheric pressure.
The high-voltage electrostatic spinning equipment in the step 3 adopts coaxial electrostatic spinning equipment, adopts a coaxial needle head with a shell layer needle cavity and a core layer needle cavity double-layer structure, the shell layer needle cavity is communicated with a shell layer injector through an injection pipe, the core layer needle cavity is communicated with the core layer injector through the injection pipe, the gel liquid is used as a core layer spinning liquid, and the semi-solidified liquid is used as a shell layer spinning liquid.
The mass ratio of the gel liquid to the semi-solidified liquid is 2:3-4, and the electrostatic spinning parameters are as follows:
the electrostatic voltage is 15-30kV, the receiving distance is 8-18cm, the advancing speed of the core layer solution is 0.05-2.0ml/h, the advancing speed of the shell layer solution is 0.1-3ml/h, and the temperature is 100-120 ℃.
The constant temperature is 100-120 ℃.
The gradient heating drying adopts two gradient heating, and specifically comprises the following steps: the temperature of the first gradient is 130-150 ℃ for 1-2h, the temperature of the second gradient is 180-190 ℃ for 3-5 h.
The pressure of the constant-temperature extrusion is 0.4-0.6MPa, and the temperature is 120-140 ℃.
Step 1, adding graphene into polypyrrole gel for ultrasonic dispersion to form a state that the graphene permeates into the polypyrrole gel, then adding distilled water into the polypyrrole gel for ultrasonic treatment to improve the softness of slurry, uniformly permeating the graphene into gel liquid, and carrying out reduced pressure distillation to obtain concentrated gel liquid.
And 2, dissolving butyl rubber in titanium tetrachloride to form a pyrolysis system, adding alumina, stirring to form a suspension state, uniformly distributing the alumina in the butyl rubber to achieve full dispersion, removing the titanium tetrachloride in a reduced pressure distillation mode to form a semi-solidified liquid, and recycling the titanium tetrachloride.
And 3, taking the gel and the semi-solidified liquid as an inner core spinning solution and a shell layer spinning solution respectively, forming the fiber yarns taking the gel liquid as an inner core in the high-pressure electrostatic spinning process, taking the semi-solidified liquid as the fiber yarns for coating the shell, gradually releasing distilled water in the inner gel liquid into a gas state along with the constant-temperature primary solidification, permeating the gas state into the semi-solidified liquid to reach a semi-solidified system, and simultaneously enabling the semi-solidified liquid to be in a solidified state and spinning to be in a single-thread shape under the characteristic action of insolubility of butyl rubber in water.
And 4, weaving the fiber yarns into the heating non-woven fabric.
Step 5, gradient heating is carried out on the heated non-woven fabric, distilled water in the graphene inner core is converted into a gaseous state in the first gradient heating process and enters the shell layer, titanium tetrachloride is converted into the gaseous state while the distilled water is converted into the gaseous state in the second gradient heating process, rapid evaporation is formed, the distilled water-titanium tetrachloride mixed waste gas is removed, and butyl rubber in the non-woven fabric shrinks; the non-woven fabrics forms the hole because of releasing the solvent and is extruded and seal in the extrusion process of constant temperature, forms compact structure, reduces inside space effect. Based on the pollution property of titanium tetrachloride, distilled water-titanium tetrachloride waste gas can be sequentially liquefied through temperature change, so that the aim of separating and recycling liquid is fulfilled, and the effect of environmental pollution is reduced.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of poor heat-insulating effect of the existing fabric, and the graphene fabric is utilized to form an electric heating system, so that a good heat-insulating effect is realized.
2. The invention utilizes a coaxial electrostatic spinning mode to form the filament with the graphene conductor as the inner core, and the filament with the heat conduction material as the outer shell to form the electrical heating-heat release integrated spinning.
3. The non-woven fabric with good connection and heat conduction effects is woven by taking the electrical heating spinning as the spinning monofilaments, the graphene fiber filaments of the inner core also have good heat conduction effects when not electrified, and the monofilaments can be used as the heat conduction spinning monofilaments.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
A preparation method of a graphene heating fabric comprises the following steps:
step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution;
step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed;
step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns;
step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric;
and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric.
The mass ratio of the graphene to the polypyrrole gel in the step 1 is 4:0.5, the adding amount of the distilled water is 300% of the mass of the graphene, the frequency of the ultrasonic wave is 40kHz, the temperature is 40 ℃, the temperature of the reduced pressure distillation is 120 ℃, the pressure is 70% of the atmospheric pressure, and the volume of the gel liquid is 20% of the volume of the solution before the reduced pressure distillation.
The concentration of the butyl rubber in the titanium tetrachloride in the step 2 is 100g/L, the stirring speed is 1000r/min, the adding amount of the alumina is 150 percent of the mass of the butyl rubber, the temperature of the reduced pressure distillation is 150 ℃, and the pressure is 80 percent of the atmospheric pressure.
The high-voltage electrostatic spinning equipment in the step 3 adopts coaxial electrostatic spinning equipment, adopts a coaxial needle head with a shell layer needle cavity and a core layer needle cavity double-layer structure, the shell layer needle cavity is communicated with a shell layer injector through an injection pipe, the core layer needle cavity is communicated with the core layer injector through the injection pipe, the gel liquid is used as a core layer spinning liquid, and the semi-solidified liquid is used as a shell layer spinning liquid.
The mass ratio of the gel liquid to the semi-solidified liquid is 2:3, and the electrostatic spinning parameters are as follows:
the electrostatic voltage is 15kV, the receiving distance is 8cm, the advancing speed of the core layer solution is 0.05ml/h, the advancing speed of the shell layer solution is 0.1ml/h, and the temperature is 100 ℃.
The constant temperature was 100 ℃.
The gradient heating drying adopts two gradient heating, and specifically comprises the following steps: the temperature of the first gradient is 130 ℃ for 1h, and the temperature of the second gradient is 180 ℃ for 3 h.
The pressure of the constant-temperature extrusion is 0.4MPa, and the temperature is 120 ℃.
Example 2
A preparation method of a graphene heating fabric comprises the following steps:
step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution;
step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed;
step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns;
step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric;
and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric.
The mass ratio of the graphene to the polypyrrole gel in the step 1 is 4:1, the adding amount of the distilled water is 450% of the mass of the graphene, the frequency of the ultrasonic wave is 80kHz, the temperature is 50 ℃, the temperature of the reduced pressure distillation is 150 ℃, the pressure is 80% of the atmospheric pressure, and the volume of the gel liquid is 30% of the volume of the solution before the reduced pressure distillation.
The concentration of the butyl rubber in the titanium tetrachloride in the step 2 is 200g/L, the stirring speed is 2000r/min, the adding amount of the alumina is 300 percent of the mass of the butyl rubber, the temperature of the reduced pressure distillation is 170 ℃, and the pressure is 90 percent of the atmospheric pressure.
The high-voltage electrostatic spinning equipment in the step 3 adopts coaxial electrostatic spinning equipment, adopts a coaxial needle head with a shell layer needle cavity and a core layer needle cavity double-layer structure, the shell layer needle cavity is communicated with a shell layer injector through an injection pipe, the core layer needle cavity is communicated with the core layer injector through the injection pipe, the gel liquid is used as a core layer spinning liquid, and the semi-solidified liquid is used as a shell layer spinning liquid.
The mass ratio of the gel liquid to the semi-solidified liquid is 2:4, and the electrostatic spinning parameters are as follows:
the electrostatic voltage is 30kV, the receiving distance is 18cm, the advancing speed of the core layer solution is 2.0ml/h, the advancing speed of the shell layer solution is 3ml/h, and the temperature is 120 ℃.
The constant temperature was 120 ℃.
The gradient heating drying adopts two gradient heating, and specifically comprises the following steps: the temperature of the first gradient is 150 ℃ and the time is 2h, and the temperature of the second gradient is 190 ℃ and the time is 5 h.
The pressure of the constant-temperature extrusion is 0.6MPa, and the temperature is 140 ℃.
Example 3
A preparation method of a graphene heating fabric comprises the following steps:
step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution;
step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed;
step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns;
step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric;
and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric.
The mass ratio of the graphene to the polypyrrole gel in the step 1 is 4:0.8, the addition amount of the distilled water is 350% of the mass of the graphene, the frequency of the ultrasonic wave is 60kHz, the temperature is 45 ℃, the temperature of the reduced pressure distillation is 140 ℃, the pressure is 75% of the atmospheric pressure, and the volume of the gel liquid is 25% of the volume of the solution before the reduced pressure distillation.
The concentration of the butyl rubber in the titanium tetrachloride in the step 2 is 150g/L, the stirring speed is 1500r/min, the adding amount of the alumina is 200 percent of the mass of the butyl rubber, the temperature of the reduced pressure distillation is 160 ℃, and the pressure is 85 percent of the atmospheric pressure.
The high-voltage electrostatic spinning equipment in the step 3 adopts coaxial electrostatic spinning equipment, adopts a coaxial needle head with a shell layer needle cavity and a core layer needle cavity double-layer structure, the shell layer needle cavity is communicated with a shell layer injector through an injection pipe, the core layer needle cavity is communicated with the core layer injector through the injection pipe, the gel liquid is used as a core layer spinning liquid, and the semi-solidified liquid is used as a shell layer spinning liquid.
The mass ratio of the gel liquid to the semi-solidified liquid is 2:3, and the electrostatic spinning parameters are as follows:
the electrostatic voltage is 24kV, the receiving distance is 12cm, the advancing speed of the core layer solution is 1.5ml/h, the advancing speed of the shell layer solution is 2ml/h, and the temperature is 110 ℃.
The constant temperature was 110 ℃.
The gradient heating drying adopts two gradient heating, and specifically comprises the following steps: the temperature of the first gradient was 140 ℃ for 2h, and the temperature of the second gradient was 185 ℃ for 4 h.
The pressure of the constant-temperature extrusion is 0.5MPa, and the temperature is 130 ℃.
Performance detection
The comparative example used a conventional electrically heated fabric, specifically arranged in accordance with the heating vest of CN 201820848625.7.
Experimental mode: 5V power supplies are added to two ends of the fabric in the embodiment 1, and temperature sensors are arranged at intervals on the bottom surface of the fabric.
Example 1 Comparative example
Temperature difference 0.2℃ 2.3℃
Rate of temperature rise 3℃/min 1℃/min
In summary, the invention has the following advantages:
1. the invention solves the problem of poor heat-insulating effect of the existing fabric, and the graphene fabric is utilized to form an electric heating system, so that a good heat-insulating effect is realized.
2. The invention utilizes a coaxial electrostatic spinning mode to form the filament with the graphene conductor as the inner core, and the filament with the heat conduction material as the outer shell to form the electrical heating-heat release integrated spinning.
3. The non-woven fabric with good connection and heat conduction effects is woven by taking the electrical heating spinning as the spinning monofilaments, the graphene fiber filaments of the inner core also have good heat conduction effects when not electrified, and the monofilaments can be used as the heat conduction spinning monofilaments.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.

Claims (8)

1. A preparation method of a graphene heating fabric is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding graphene into polypyrrole gel, performing ultrasonic dispersion uniformly, adding distilled water, performing continuous ultrasonic treatment until slurry is formed, and performing reduced pressure distillation to obtain a gel solution;
step 2, adding butyl rubber into titanium tetrachloride, uniformly stirring until the butyl rubber is dissolved, then adding alumina, uniformly stirring to form a suspension, and carrying out reduced pressure distillation until a semi-solidified liquid is formed;
step 3, putting the gel solution and the semi-solidified solution into high-voltage electrostatic spinning equipment for core-shell double-layer spinning, and keeping the temperature constant until the gel solution and the semi-solidified solution are primarily solidified to obtain core-shell fiber yarns;
step 4, weaving the core-shell fiber yarns to form a heating non-woven fabric;
and 5, putting the heated non-woven fabric into a reaction kettle, heating and drying the non-woven fabric in a gradient manner, and extruding the non-woven fabric at constant temperature to obtain the graphene heating fabric.
2. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the mass ratio of the graphene to the polypyrrole gel in the step 1 is 4:0.5-1, the adding amount of the distilled water is 300-450% of the mass of the graphene, the frequency of the ultrasonic is 40-80kHz, the temperature is 40-50 ℃, the temperature of the reduced pressure distillation is 120-150 ℃, the pressure is 70-80% of the atmospheric pressure, and the volume of the gel liquid is 20-30% of the solution before the reduced pressure distillation.
3. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the concentration of the butyl rubber in the step 2 in the titanium tetrachloride is 100-200g/L, the stirring speed is 1000-2000r/min, the adding amount of the alumina is 150-300% of the mass of the butyl rubber, the temperature of the reduced pressure distillation is 150-170 ℃, and the pressure is 80-90% of the atmospheric pressure.
4. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the high-voltage electrostatic spinning equipment in the step 3 adopts coaxial electrostatic spinning equipment, adopts a coaxial needle head with a shell layer needle cavity and a core layer needle cavity double-layer structure, the shell layer needle cavity is communicated with a shell layer injector through an injection pipe, the core layer needle cavity is communicated with the core layer injector through the injection pipe, the gel liquid is used as a core layer spinning liquid, and the semi-solidified liquid is used as a shell layer spinning liquid.
5. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the mass ratio of the gel liquid to the semi-solidified liquid is 2:3-4, and the electrostatic spinning parameters are as follows:
the electrostatic voltage is 15-30kV, the receiving distance is 8-18cm, the advancing speed of the core layer solution is 0.05-2.0ml/h, the advancing speed of the shell layer solution is 0.1-3ml/h, and the temperature is 100-120 ℃.
6. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the constant temperature is 100-120 ℃.
7. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the gradient heating drying adopts two gradient heating, and specifically comprises the following steps: the temperature of the first gradient is 130-150 ℃ for 1-2h, the temperature of the second gradient is 180-190 ℃ for 3-5 h.
8. The preparation method of the graphene heating fabric according to claim 1, characterized by comprising the following steps: the pressure of the constant-temperature extrusion is 0.4-0.6MPa, and the temperature is 120-140 ℃.
CN201911066302.8A 2019-11-04 2019-11-04 Preparation method of graphene heating fabric Active CN110747580B (en)

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