CN117098262B - Graphene-based snow melting heating cable and processing technology thereof - Google Patents
Graphene-based snow melting heating cable and processing technology thereof Download PDFInfo
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/40—Heating elements having the shape of rods or tubes
- H05B3/54—Heating elements having the shape of rods or tubes flexible
- H05B3/56—Heating cables
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of cables, in particular to a snow melting heating cable based on graphene and a processing technology thereof. The graphene composite material comprises the following components in parts by weight: 40-60 parts of silicon rubber, 20-30 parts of styrene-butadiene rubber, 3-5 parts of three-dimensional graphite aerogel, 5-10 parts of flame retardant, 4-8 parts of curing agent and 5-10 parts of diluent. According to the invention, the snow melting heating cable is prepared by adopting the processes of extrusion, wrapping and the like, and has excellent heat conducting performance, and meanwhile, the addition of the flame retardant endows the cable with excellent flame retardant performance.
Description
Technical Field
The invention relates to the technical field of cables, in particular to a snow melting heating cable based on graphene and a processing technology thereof.
Background
The snow melting heating cable based on graphene is a novel cable for realizing a snow melting effect by utilizing excellent electrical conductivity and thermal conductivity of a graphene material, and can be used for solving the problem of road icing in winter. Graphene is used as a novel two-dimensional material, has extremely high electrical conductivity and thermal conductivity, has excellent mechanical property and chemical stability, and can convert electric energy into heat energy, so that the road surface is kept warm, and snow accumulation and ice formation are prevented.
However, the technology still faces some challenges. Firstly, graphene is easy to oxidize at high temperature, the conductivity and the service life of the graphene are affected, and in order to solve the problem, the oxidation resistance of the graphene can be improved by controlling the chemical composition and the structure of the graphene, so that the service life of the graphene is prolonged. Meanwhile, the conductivity of the graphene is greatly influenced by factors such as temperature, strain and the like, the stability and the reliability of the graphene need to be improved by optimizing a material structure and a processing technology, the conductivity and the stability of the graphene can be improved by adopting a multi-layer graphene structure, and the mechanical property and the durability of the graphene can also be improved by filling the proper material between layers. In addition, the stability and the reliability of the graphene can be improved by optimizing the structural design and the processing technology of the cable, and the normal operation of the graphene in a severe environment can be ensured.
Therefore, we propose a graphene-based snow melting heating cable and a processing technology thereof.
Disclosure of Invention
The invention aims to provide a graphene-based snow melting heating cable and a processing technology thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a processing technology of a snow melting heating cable based on graphene comprises the following steps:
s1: respectively carrying out vacuum drying on silicon rubber and styrene-butadiene rubber for 12-24 hours, stirring for 40-50 minutes at 120-140 ℃, adding a flame retardant, a curing agent, a diluent and three-dimensional graphene aerogel for blending after uniformly mixing to obtain a mixture, adding the mixture into a double-screw extruder, extruding at 200-240 ℃, cooling, drying, cutting and granulating to obtain a graphene composite material; extruding the graphene composite material on the outer side of the heating conductor to form a conductive layer;
s2: extruding an insulating material on the outer side of the conductive layer to form an insulating layer;
s3: wrapping the copper strips on the outer semi-conductive shielding layer to form a shielding layer;
s4: and extruding and wrapping the polyvinyl chloride sheath material on the outer side of the shielding layer to form an outer protective layer, and cooling to room temperature to obtain the graphene-based snow melting heating cable.
Further, the graphene composite material comprises the following components in parts by weight: the graphene composite material comprises the following components in parts by weight: 40-60 parts of silicon rubber, 20-30 parts of styrene-butadiene rubber, 3-5 parts of three-dimensional graphite aerogel, 5-10 parts of flame retardant, 4-8 parts of curing agent and 5-10 parts of diluent
Further, the preparation method of the three-dimensional graphene aerogel comprises the following steps:
and (3) ultrasonically dispersing graphene oxide in deionized water, adding ethylenediamine, uniformly mixing, performing ultrasonic dispersion under ice bath conditions for 1-3 times, heating to 120-180 ℃, performing hydrothermal reaction for 10-12 hours, cooling to room temperature, performing hydroalcoholic dialysis, freeze drying, and performing heat treatment at 200-500 ℃ for 1-2 hours in an argon atmosphere to obtain the three-dimensional graphene aerogel.
Further, the mass ratio of the graphene oxide to the deionized water is 1: (500-1000).
Further, the ultrasonic dispersion process conditions are as follows: the ultrasonic time is 2-3h, and the ultrasonic power is 500-600W.
Further, the mass of the ethylenediamine is 0.4-0.6% of the total mass of the graphene oxide and the deionized water.
In the technical scheme, graphene oxide is used as a raw material, ethylenediamine is used as a nitrogen source, the three-dimensional graphene aerogel with high nitrogen content is prepared through a hydrothermal method, flexible graphene sheets are connected with each other to form a three-dimensional porous structure, the unique three-dimensional porous structure can prevent the graphene sheets from being stacked in parallel, electrolyte ions can be freely transmitted in an internal three-dimensional network structure, and the three-dimensional graphene aerogel has the advantages of being high in specific surface area, excellent in conductivity, good in mechanical property, high in heat conducting property, adjustable and the like.
Further, the preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 1,3, 5-triglycidyl-S-triazinetrione and methacrylic acid, adding triethylamine and p-hydroxyanisole, heating to 100-110 ℃, reacting for 3-4 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, uniformly mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and a double bond-containing compound A, heating to 80-90 ℃, reacting for 2-3 hours, adding methyltrimethoxysilane and toluene, uniformly mixing, adding a Caster catalyst, heating to 95-105 ℃, carrying out reflux reaction for 6-8 hours, and carrying out rotary steaming, washing and drying to obtain the flame retardant.
In the technical scheme, by taking triethylamine as a catalyst and P-hydroxyanisole as a polymerization inhibitor, ring-opening reaction is carried out on epoxy groups in 1,3, 5-triglycidyl-S-triazinetrione and carbon-carbon double bonds of methacrylic acid to generate a compound A containing 3 carbon-carbon double bonds, P-H bonds in 2mol of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 2mol of carbon-carbon double bonds in the compound A can be subjected to addition reaction, P element is introduced, methyltrimethoxysilane and the rest 1mol of carbon-carbon double bonds are reacted, si element is introduced, and a N, P, si element-containing flame retardant is prepared, wherein N, P, si element can be in synergistic effect at high temperature and react with free radicals in combustion products to form a stable nitrogen, phosphorus and silicon oxide layer, so that the combustion reaction is prevented from being carried out, and the flame retardant effect is achieved; the three-dimensional graphite aerogel is used as the filler, the silicon rubber and the styrene-butadiene rubber are used as the base materials, and the mutual contact of the filler in the polymer base materials is increased by combining the combined action of the flame retardant, the curing agent and the diluent, so that the density of the heat conducting network is effectively improved, and meanwhile, the flame retardant performance of the material is enhanced by adding the flame retardant.
Further, in the step (1), the mass ratio of the 1,3, 5-triglycidyl-S-triazinetrione to the methacrylic acid is 1: (0.9-1.2).
Further, the mass of the triethylamine in the step (1) is 0.7-1.0% of the mass of the 1,3, 5-triglycidyl-S-triazinetrione.
Further, the mass of the para-hydroxyanisole in the step (1) is 1-3% of the mass of the 1,3, 5-triglycidyl-S-triazinetrione.
Further, in the step (2), the mass ratio of the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to the double bond-containing compound A is 1: (1.2-1.4).
Further, in the step (2), the mass ratio of methyltrimethoxysilane to toluene is 1: (4-6).
Further, the mass of methyltrimethoxysilane in the step (2) is 14-16% of the total mass of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and double bond-containing compound A.
Further, the mass of the Kasite catalyst in the step (2) is 6-8ppm of the mass of methyltrimethoxysilane.
Further, the diluent is propylene glycol methyl ether.
Further, the heating conductor is formed by twisting 2-4 strands of ferrochrome wires and 2-5 strands of nichrome wires.
Further, the insulating material is chlorosulfonated polyethylene.
Further, the thickness of the conductive layer is 0.5-1.5mm.
Further, the thickness of the insulating layer is 3-5mm.
Further, the thickness of the shielding layer is 0.8-1.2mm.
Further, the thickness of the outer protective layer is 1.0-2.0mm.
Further, the temperature of the extrusion process is 250-350 ℃.
Further, the construction process of the snow melting heating cable based on the graphene specifically comprises the following steps:
a. preparation: before construction, the road needs to be cleaned and checked, so that the road surface is smooth and no obvious damage or crack exists;
b. laying a heat insulation layer: using polystyrene foam plate as heat insulating layer with thickness of 30-40mm;
c. laying composite aluminum foil cloth and steel wire mesh: the composite aluminum foil cloth is fixedly stuck with the heat insulation layer, and the joint is firmly stuck by an aluminum foil tape; laying a steel wire mesh on the composite aluminum foil cloth, wherein the steel wire mesh adopts argon arc welding steel wire meshes with phi 2.0-3.5mm and meshes of 100mm multiplied by 100mm, and the steel wire mesh connection is bound by a binding belt;
d. wiring and mounting: five heating cables are connected through a K-shaped connector and then connected in parallel to a cold wire to form a group; the pavement power is 250-400W/m according to the direction of the vertical pavement mode 2 Wiring is performed, and the laying pitch is calculated by the following formula: lay pitch (mm) =heating cable power per meter/heating cable power to install per square meter x 1000, or pitch (mm) =real area/heating cable length x 1000; binding the heating cable on the steel wire net by using a binding belt, wherein the distance between binding fixed points is generally 0.5-0.7m, and the distance between binding fixed points is 0.2-0.3 m;
e. connection and test: connecting a power line of the heating cable with a power system, ensuring firm connection and performing electrical test to verify the normal working state of the product;
f. and (3) filling layer construction: and C15 pea stone concrete (with the grain diameter of 5-12 mm) is used for covering and protecting the heating cable to form a filling layer, and the thickness of the filling layer is 35-45mm.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the graphene-based snow-melting heating cable and the processing technology thereof, the three-dimensional graphene aerogel with high nitrogen content is prepared by a hydrothermal method, and flexible graphene sheets are connected with each other to form a three-dimensional porous structure, so that the unique three-dimensional porous structure can not only prevent the graphene sheets from being stacked in parallel, but also enable electrolyte ions to be freely transmitted in an internal three-dimensional network structure, and has the advantages of high specific surface area, excellent conductivity, good mechanical property, high heat-conducting property, adjustability and the like; the epoxy group in 1,3, 5-triglycidyl-S-triazinetrione and the carbon-carbon double bond of methacrylic acid are subjected to ring opening reaction to generate a compound A containing 3 carbon-carbon double bonds, P-H bonds in 2mol of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide are subjected to addition reaction with 2mol of carbon-carbon double bonds in the compound A, P element is introduced, methyltrimethoxysilane is reacted with the rest 1mol of carbon-carbon double bonds, si element is introduced, a flame retardant containing N, P, si element is prepared, N, P, si elements can synergistically react with free radicals in combustion products at high temperature to form a stable nitrogen, phosphorus and silicon oxide layer, so that the combustion reaction is prevented, and the flame retardant effect is achieved; the three-dimensional graphite aerogel is used as the filler, the silicon rubber and the styrene-butadiene rubber are used as the base materials, and the mutual contact of the filler in the polymer base materials is increased by combining the combined action of the flame retardant, the curing agent and the diluent, so that the density of the heat conducting network is effectively improved, and meanwhile, the flame retardant performance of the material is enhanced by adding the flame retardant.
2. According to the graphene-based snow melting heating cable and the processing technology thereof, the iron-chromium alloy wire and the nickel-chromium alloy wire are stranded to form the heating conductor, the iron-chromium alloy wire has high electrical conductivity and thermal conductivity, good current conduction and heat transfer can be provided, the nickel-chromium alloy wire has high corrosion resistance and high temperature resistance, the cable can stably work in a complex environment, and a uniform and stable heat conducting network can be formed by stranding the two alloy wires together, so that the overall heat conducting performance is improved; the graphene composite material is used as the conductive layer for melting snow or ice covered on a road or other surfaces, so that the traffic capacity and safety of the road are effectively improved, and traffic accidents are reduced; the chlorosulfonated polyethylene is used as the insulating layer, so that the conducting layer and the outer semi-conducting shielding layer can be effectively isolated, electric energy leakage and loss are prevented, and the safety performance of the cable is improved; the copper strip wrapping is used as a shielding layer, so that the external electromagnetic interference can be effectively shielded, and the cable is prevented from being interfered to influence the normal work; the polyvinyl chloride sheath material is used as an outer protective layer to provide additional protection to prevent the cable from physical damage and environmental erosion. Through the combination of the structure and the materials, heat can be quickly and uniformly generated, the heat-conducting performance and the protection performance are good, and the heat-conducting composite material is suitable for various places needing snow melting functions, such as roads, bridges, parking lots and the like.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Graphene oxide in this embodiment: DN-20WY, average thickness of 1-3nm, diameter of 4-7 μm, number of layers of 2-5, carbon content of more than or equal to 99wt%, sulfur content of less than or equal to 0.5%, and is from Zhejiang Zhi Tina micro new material Co; silicone rubber: 107 silicone rubber from Jinan first pass chemical technology limited company; curing agent: the YX-GHJ silica gel curing agent is derived from Shenzhen New technology Co., ltd; iron-chromium alloy wire: the brand of 0Cr25Al5, the wire diameter of 0.15-0.30mm, is from Jiangsu wear of the communication technology Co., ltd; twisting nickel-chromium alloy wires: germany BGH Ni80Cr20, wire diameter 0.4mm, from the company of constant electric heating technology, inc. In salt city; chlorosulfonated polyethylene: CSM40, with an average molecular weight of 40000, is derived from the company of the petrochemical industry Co., ltd; polyvinyl chloride sheath material: the brand PVC5 is from Sanzhuang plastic products limited company in Kaisha county; in the following specific embodiments, the thicknesses of the conductive layers are 1.0mm, the insulating layers are 4mm, the outer semiconductive shielding layers are 1.2mm, the shielding layers are 1.0mm, and the outer protective layers are 1.5mm.
The following examples and comparative examples equal 10g in 1 serving.
Example 1: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
s1: respectively carrying out vacuum drying on 40 parts of silicon rubber and 20 parts of styrene-butadiene rubber for 12 hours, stirring for 40 minutes at 120 ℃, adding 5 parts of flame retardant, 4 parts of curing agent, 5 parts of diluent and 3 parts of three-dimensional graphene aerogel for blending to obtain a mixture, adding the mixture into a double-screw extruder, extruding at 200 ℃, cooling, drying, cutting and granulating to obtain a graphene composite material; extruding the graphene composite material on the outer side of a heating conductor (formed by twisting 2 strands of ferrochrome wires and 5 strands of nichrome wires) to form a conductive layer;
s2: extruding chlorosulfonated polyethylene on the outer side of the conductive layer to form an insulating layer;
s3: wrapping the copper strips on the outer semi-conductive shielding layer to form a shielding layer;
s4: extruding polyvinyl chloride sheath material on the outer side of the shielding layer to form an outer protective layer, and cooling to room temperature to obtain the graphene-based snow-melting heating cable;
the preparation method of the three-dimensional graphene aerogel comprises the following steps:
3 parts of graphene oxide is ultrasonically dispersed in 1500 parts of deionized water (ultrasonic time is 2h, ultrasonic power is 500W), 6 parts of ethylenediamine is added and uniformly mixed, ultrasonic dispersion is carried out under ice bath conditions (ultrasonic time is 2h, ultrasonic power is 500W), ultrasonic is carried out for 1 time, temperature is increased to 120 ℃, hydrothermal reaction is carried out for 10h, cooling is carried out to room temperature, and after hydroalcoholic dialysis and freeze drying, heat treatment is carried out for 1h at 200 ℃ under argon atmosphere, so that three-dimensional graphene aerogel is prepared;
the preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 10 parts of 1,3, 5-triglycidyl-S-triazinetrione and 9 parts of methacrylic acid, adding 0.07 part of triethylamine and 0.1 part of p-hydroxyanisole, heating to 100 ℃, reacting for 3 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, 10 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 12 parts of double bond-containing compound A are uniformly mixed, heated to 80 ℃, reacted for 2 hours, 3.08 parts of methyltrimethoxysilane and 12.32 parts of toluene are added, uniformly mixed, 6ppm of Kanster catalyst is added, heated to 95 ℃, refluxed and reacted for 6 hours, and the flame retardant is prepared after rotary steaming, washing and drying.
Example 2: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
s1: respectively carrying out vacuum drying on 50 parts of silicon rubber and 25 parts of styrene-butadiene rubber for 18 hours, stirring for 45 minutes at 130 ℃, adding 8 parts of flame retardant, 6 parts of curing agent, 8 parts of diluent and 4 parts of three-dimensional graphene aerogel for blending to prepare a mixture, adding the mixture into a double-screw extruder, extruding at 220 ℃, cooling, drying, cutting and granulating to prepare the graphene composite material; extruding the graphene composite material on the outer side of a heating conductor (formed by twisting 3 strands of ferrochrome wires and 4 strands of nichrome wires) to form a conductive layer;
s2: extruding chlorosulfonated polyethylene on the outer side of the conductive layer to form an insulating layer;
s3: wrapping the copper strips on the outer semi-conductive shielding layer to form a shielding layer;
s4: extruding polyvinyl chloride sheath material on the outer side of the shielding layer to form an outer protective layer, and cooling to room temperature to obtain the graphene-based snow-melting heating cable;
the preparation method of the three-dimensional graphene aerogel comprises the following steps:
4 parts of graphene oxide is ultrasonically dispersed in 2800 parts of deionized water (ultrasonic time is 2.5h, ultrasonic power is 550W), 14 parts of ethylenediamine is added and uniformly mixed, ultrasonic dispersion is carried out under ice bath conditions (ultrasonic time is 2.5h, ultrasonic power is 550W), ultrasonic is carried out for 2 times, temperature is increased to 150 ℃, hydrothermal reaction is carried out for 11h, cooling is carried out to room temperature, and after hydroalcoholic dialysis and freeze drying, heat treatment is carried out for 1.5h at 300 ℃ under argon atmosphere, thus obtaining the three-dimensional graphene aerogel.
The preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 10 parts of 1,3, 5-triglycidyl-S-triazinetrione and 10 parts of methacrylic acid, adding 0.08 part of triethylamine and 0.2 part of p-hydroxyanisole, heating to 105 ℃, reacting for 3.5 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, 10 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 13 parts of double bond-containing compound A are uniformly mixed, heated to 85 ℃, reacted for 2.5 hours, 3.45 parts of methyltrimethoxysilane and 17.25 parts of toluene are added, uniformly mixed, 7ppm of Kanster catalyst is added, heated to 100 ℃, refluxed for 7 hours, and subjected to rotary evaporation, washing and drying to obtain the flame retardant.
Example 3: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
s1: respectively carrying out vacuum drying on 60 parts of silicon rubber and 30 parts of styrene-butadiene rubber for 24 hours, stirring for 50 minutes at 140 ℃, adding 10 parts of flame retardant, 8 parts of curing agent, 10 parts of diluent and 5 parts of three-dimensional graphene aerogel for blending to obtain a mixture, adding the mixture into a double-screw extruder, extruding at 240 ℃, cooling, drying, cutting and granulating to obtain a graphene composite material; extruding the graphene composite material on the outer side of a heating conductor (formed by twisting 4 strands of ferrochrome wires and 2 strands of nichrome wires) to form a conductive layer;
s2: extruding chlorosulfonated polyethylene on the outer side of the conductive layer to form an insulating layer;
s3: wrapping the copper strips on the outer semi-conductive shielding layer to form a shielding layer;
s4: extruding polyvinyl chloride sheath material on the outer side of the shielding layer to form an outer protective layer, and cooling to room temperature to obtain the graphene-based snow-melting heating cable;
the preparation method of the three-dimensional graphene aerogel comprises the following steps:
dispersing 5 parts of graphene oxide in 5000 parts of deionized water ultrasonically (ultrasonic time is 3h, ultrasonic power is 600W), adding 30 parts of ethylenediamine, uniformly mixing, performing ultrasonic dispersion under ice bath conditions (ultrasonic time is 3h, ultrasonic power is 600W), performing ultrasonic treatment for 3 times, heating to 180 ℃, performing hydrothermal reaction for 12h, cooling to room temperature, performing hydroalcoholic dialysis, freeze drying, and performing heat treatment at 500 ℃ for 2h under argon atmosphere to obtain three-dimensional graphene aerogel;
the preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 10 parts of 1,3, 5-triglycidyl-S-triazinetrione and 12 parts of methacrylic acid, adding 0.1 part of triethylamine and 0.3 part of p-hydroxyanisole, heating to 110 ℃, reacting for 4 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, 10 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 14 parts of double bond-containing compound A are uniformly mixed, heated to 90 ℃, reacted for 3 hours, 3.84 parts of methyltrimethoxysilane and 23.04 parts of toluene are added, uniformly mixed, 8ppm of Kanster catalyst is added, heated to 105 ℃, refluxed and reacted for 8 hours, and the flame retardant is prepared after spin steaming, washing and drying.
Comparative example 1: the graphene composite material comprises the following components in parts by weight: 40 parts of silicon rubber, 20 parts of styrene-butadiene rubber, 5 parts of flame retardant, 4 parts of curing agent, 5 parts of propylene glycol methyl ether and 0.5 part of three-dimensional graphite aerogel, and the other steps and processes are the same as in example 1.
Comparative example 2: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
in comparison with example 1, comparative example 2 was omitted from the graphene composite preparation method, the graphene composite in step S1 was replaced with a crosslinked polyethylene material (HDPE single mountain petrochemical 8008H, derived from shanghai bang tao international trade company), and the other steps were the same as in example 1.
Comparative example 3: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
in comparison with example 2, comparative example 3 was omitted in the preparation method of the flame retardant, the flame retardant in step S1 was replaced with an ammonium polyphosphate of the same quality (originating from Ji-nan Xin Nuo chemical Co., ltd.), and the other steps were the same as in example 2.
Comparative example 4: a processing technology of a snow melting heating cable based on graphene comprises the following steps:
the preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 10 parts of 1,3, 5-triglycidyl-S-triazinetrione and 5 parts of methacrylic acid, adding 0.08 part of triethylamine and 0.2 part of p-hydroxyanisole, heating to 105 ℃, reacting for 3.5 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, uniformly mixing 10 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and 13 parts of double bond-containing compound A, heating to 85 ℃, reacting for 2.5 hours, adding 3.45 parts of methyltrimethoxysilane and 17.25 parts of toluene, uniformly mixing, adding 7ppm of Kanster catalyst, heating to 100 ℃, refluxing for 7 hours, and preparing the flame retardant after rotary steaming, washing and drying;
in comparison with example 2, the mass ratio of 1,3, 5-triglycidyl-S-triazinetrione to methacrylic acid in comparative example 4 is 1:0.5; the remaining steps were the same as in example 2.
Experiment
Taking the graphene-based snow-melting heating cables obtained in examples 1-3 and comparative examples 1-4, preparing samples, respectively detecting the performances of the samples and recording detection results:
according to GB/T18380.11-2022 section 11, combustion test of electric and optical cables under flame conditions: the flame retardant property of a single insulated wire and cable flame vertical spreading test device is measured, and the test steps are as follows: the length of the sample is 600mm, the width is 50mm, the thickness is more than or equal to 1.5mm, the sample is fixed on a testing device, the sample is ignited, and the burning starting time of the sample and various parameters in the burning process are recorded. Class a: without vertical combustion propagation (highest ranking), the flame cannot propagate upwards in the vertical direction; class B1: the vertical combustion propagation speed is less than or equal to 40mm/min, and the flame upward spreading speed along the vertical direction is not more than 40mm/min; class B2: the vertical combustion propagation speed is less than or equal to 265mm/min, and the flame upward spreading speed in the vertical direction is not more than 265mm/min; class B3: the vertical combustion propagation speed is less than or equal to 425mm/min, and the flame propagation speed in the vertical direction is not more than 425mm/min.
The graphene composite materials of examples 1 to 3 and comparative examples 1,3 and 4 and the crosslinked polyethylene material of comparative example 2 were respectively prepared into sample pieces with a thickness of 0.2mm, and the thermal conductivity at 80 ℃ was measured by using a laser flash thermal conductivity meter, and the average value was obtained three times.
Test results
From the data in the above table, the following conclusions can be clearly drawn:
1. compared with the embodiment 1-3, the thermal conductivity of the product obtained in the comparative example 1 is reduced, which shows that the thermal conductivity of the graphene composite material prepared by the method is influenced by the proportion of each component in the preparation process, and the mass proportion within the range is selected, so that the prepared material has excellent thermal conductivity.
2. Compared with examples 1-3, the flame retardant property and the heat conductivity coefficient of the product obtained in the comparative example 2 are reduced, which shows that the graphene composite material prepared by the invention has better flame retardant property and heat conductivity compared with the crosslinked polyethylene material; the flame retardant performance of the product obtained in the comparative example 3 is reduced, and compared with ammonium polyphosphate, the flame retardant prepared by the invention has better flame retardant effect and can improve the flame retardant performance of the material.
3. Compared with examples 1-3, the flame retardant property of the product obtained in comparative example 4 is reduced, which shows that the flame retardant property of the graphene composite material prepared by the invention is influenced by the ratio of each reagent in the preparation process, and the mass ratio in the range is selected, so that the prepared material has excellent flame retardant property, and the service life of the material is prolonged.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The processing technology of the snow melting heating cable based on the graphene is characterized by comprising the following steps of: the method comprises the following steps:
s1: respectively carrying out vacuum drying on silicon rubber and styrene-butadiene rubber for 12-24 hours, stirring for 40-50 minutes at 120-140 ℃, adding a flame retardant, a curing agent, a diluent and three-dimensional graphene aerogel for blending after uniformly mixing to obtain a mixture, adding the mixture into a double-screw extruder, extruding at 200-240 ℃, cooling, drying, cutting and granulating to obtain a graphene composite material; extruding the graphene composite material on the outer side of the heating conductor to form a conductive layer;
s2: extruding an insulating material on the outer side of the conductive layer to form an insulating layer;
s3: wrapping the copper strips on the outer semi-conductive shielding layer to form a shielding layer;
s4: extruding polyvinyl chloride sheath material on the outer side of the shielding layer to form an outer protective layer, and cooling to room temperature to obtain the graphene-based snow-melting heating cable;
the graphene composite material comprises the following components in parts by weight: 40-60 parts of silicon rubber, 20-30 parts of styrene-butadiene rubber, 3-5 parts of three-dimensional graphite aerogel, 5-10 parts of flame retardant, 4-8 parts of curing agent and 5-10 parts of diluent;
the preparation method of the three-dimensional graphene aerogel comprises the following steps:
dispersing graphene oxide in deionized water by ultrasonic, adding ethylenediamine, uniformly mixing, performing ultrasonic dispersion under ice bath conditions for 1-3 times, heating to 120-180 ℃, performing hydrothermal reaction for 10-12 hours, cooling to room temperature, performing dialysis and freeze drying, and performing heat treatment for 1-2 hours at 200-500 ℃ under argon atmosphere to obtain three-dimensional graphene aerogel;
the preparation method of the flame retardant comprises the following steps:
step (1): uniformly mixing 1,3, 5-triglycidyl-S-triazinetrione and methacrylic acid, adding triethylamine and p-hydroxyanisole, heating to 100-110 ℃, reacting for 3-4 hours, and performing rotary evaporation to obtain a double bond-containing compound A;
step (2): under the protection of nitrogen, uniformly mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and a double bond-containing compound A, heating to 80-90 ℃, reacting for 2-3 hours, adding methyltrimethoxysilane and toluene, uniformly mixing, adding a Caster catalyst, heating to 95-105 ℃, carrying out reflux reaction for 6-8 hours, and carrying out rotary steaming, washing and drying to obtain the flame retardant.
2. The processing technology of the graphene-based snow melting heating cable according to claim 1, wherein the processing technology is characterized in that: the ultrasonic dispersion process conditions are as follows: the ultrasonic time is 2-3h, and the ultrasonic power is 500-600W.
3. The processing technology of the graphene-based snow melting heating cable according to claim 1, wherein the processing technology is characterized in that: the mass ratio of the 1,3, 5-triglycidyl-S-triazinetrione to the methacrylic acid in the step (1) is 1: (0.9-1.2).
4. The processing technology of the graphene-based snow melting heating cable according to claim 1, wherein the processing technology is characterized in that: the heating conductor is formed by twisting 2-4 strands of ferrochrome wires and 2-5 strands of nichrome wires.
5. The processing technology of the graphene-based snow melting heating cable according to claim 1, wherein the processing technology is characterized in that: the insulating material is chlorosulfonated polyethylene.
6. The processing technology of the graphene-based snow melting heating cable according to claim 1, wherein the processing technology is characterized in that: the temperature of the extrusion process is 250-350 ℃.
7. A graphene-based snow-melting heating cable produced by the process of any one of claims 1-6.
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