CN116656033B - Graphene-containing stretch-resistant polyethylene cable material and preparation process thereof - Google Patents
Graphene-containing stretch-resistant polyethylene cable material and preparation process thereof Download PDFInfo
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- CN116656033B CN116656033B CN202310406918.5A CN202310406918A CN116656033B CN 116656033 B CN116656033 B CN 116656033B CN 202310406918 A CN202310406918 A CN 202310406918A CN 116656033 B CN116656033 B CN 116656033B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000463 material Substances 0.000 title claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 50
- 239000004698 Polyethylene Substances 0.000 title claims abstract description 35
- -1 polyethylene Polymers 0.000 title claims abstract description 35
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 20
- 229920000092 linear low density polyethylene Polymers 0.000 claims abstract description 15
- 239000004707 linear low-density polyethylene Substances 0.000 claims abstract description 15
- 229920003048 styrene butadiene rubber Polymers 0.000 claims abstract description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 11
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 11
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008187 granular material Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 76
- 238000006243 chemical reaction Methods 0.000 claims description 66
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000007795 chemical reaction product Substances 0.000 claims description 29
- 239000012153 distilled water Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 18
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 16
- 239000011246 composite particle Substances 0.000 claims description 15
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 230000001376 precipitating effect Effects 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- DKCPKDPYUFEZCP-UHFFFAOYSA-N 2,6-di-tert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=C1O DKCPKDPYUFEZCP-UHFFFAOYSA-N 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- QXJCOPITNGTALI-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,4-nonafluorobutan-1-ol Chemical compound OC(F)(F)C(F)(F)C(F)(F)C(F)(F)F QXJCOPITNGTALI-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- 238000007792 addition Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 2
- 230000009471 action Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 238000010992 reflux Methods 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000002390 rotary evaporation Methods 0.000 description 6
- 239000005543 nano-size silicon particle Substances 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 125000001246 bromo group Chemical group Br* 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000001263 acyl chlorides Chemical group 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/14—Extreme weather resilient electric power supply systems, e.g. strengthening power lines or underground power cables
Abstract
The invention relates to the field of cable materials, in particular to a graphene-containing stretch-resistant polyethylene cable material and a preparation process thereof, which are used for solving the problem that the existing polyethylene cable material is poor in stretch resistance; adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and an antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying granules to obtain the graphene-containing stretch-resistant polyethylene cable material; in the preparation process, the linear low-density polyethylene and the styrene-butadiene rubber are used as main raw materials, and the reinforcing filler is added into the linear low-density polyethylene and the styrene-butadiene rubber, so that the tensile resistance of the cable material can be greatly improved, the cable can not be easily damaged under the action of external force, and potential safety hazards are avoided.
Description
Technical Field
The invention relates to the field of cable materials, in particular to a graphene-containing stretch-resistant polyethylene cable material and a preparation process thereof.
Background
The cable is typically a rope-like cable formed by twisting at least two wires of each group of several or groups of wires, each group of wires being insulated from each other and often twisted around a center, the whole being covered with a highly insulating coating. The wire and cable industry is a matching industry of the power industry which is one of national economy supporting industry, and has extremely important roles and positions in national economy.
The polyethylene cable material has the incomparable advantages of the PVC cable material, and has the advantages of light weight, good heat resistance, strong loading capacity, chemical corrosion resistance and high mechanical strength, and is widely applied to power distribution networks, industrial devices or other fields requiring large-capacity electricity. However, with the expansion of the application occasions of wires and cables, the requirements on polyethylene cable sheath materials are continuously improved, some cables are often laid outdoors in a high-altitude erection mode, and the cables can generate acting force to the materials to cause material damage and potential safety hazards due to the influence of gravity in the past, so that the tensile strength of the common polyethylene cable sheath materials in the market at present cannot meet the market requirements.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a graphene-containing stretch-resistant polyethylene cable material and a preparation process thereof: the graphene-containing stretch-resistant polyethylene cable material is prepared by adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying the granules.
The aim of the invention can be achieved by the following technical scheme:
a preparation process of a graphene-containing stretch-resistant polyethylene cable material comprises the following steps:
step one: 15-20 parts of linear low-density polyethylene, 5-9 parts of styrene-butadiene rubber, 2-12 parts of reinforcing filler, 7-13 parts of polyvinyl alcohol, 0.8-1.4 parts of zinc stearate and 0.4-0.6 part of antioxidant are weighed according to parts by weight for standby;
step two: adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying the granules to obtain the graphene-containing stretch-resistant polyethylene cable material.
As a further scheme of the invention: the reinforcing filler is prepared by the following steps:
step A1: adding 2, 6-di-tert-butylphenol, sodium hydroxide, deionized water, toluene and N, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 20-30 min under the conditions of 25-30 ℃ and stirring speed of 500-600 r/min, heating to reflux, continuing stirring and reacting until no moisture is separated out, introducing carbon dioxide gas under the conditions of 100-110 ℃ and pressure of 0.65-0.7MPa until the reaction system does not absorb carbon dioxide gas any more, cooling the reaction product to room temperature after the reaction is finished, adding into distilled water, adjusting the pH to 1-2 by using concentrated hydrochloric acid, precipitating, performing vacuum suction filtration, washing a filter cake with distilled water for 3-5 times, placing in a vacuum drying box, and drying for 2-3h under the conditions of 70-75 ℃ to obtain an intermediate 1;
the reaction principle is as follows:
step A2: adding the intermediate 1, thionyl chloride and N, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 5-10 min under the conditions that the temperature is 25-30 ℃ and the stirring speed is 500-600 r/min, heating to reflux, continuing stirring and reacting for 5-6h, cooling the reaction product to room temperature after the reaction is finished, and removing redundant thionyl chloride by rotary evaporation to obtain an intermediate 2;
the reaction principle is as follows:
step A3: adding the intermediate 2, N-bromosuccinimide and N, N-dimethylformamide into a three-neck flask with a stirrer and a thermometer, stirring and reacting for 1-1.5 hours under the conditions that the temperature is-5-0 ℃ and the stirring speed is 500-600 r/min, then heating to 35-40 ℃ and continuously stirring and reacting for 10-15 hours, adding the reaction product into distilled water after the reaction is finished, precipitating and precipitating, then vacuum filtering, and recrystallizing a filter cake with acetone to obtain an intermediate 3;
the reaction principle is as follows:
step A4: adding the intermediate 3, composite particles, triethylamine and N, N-dimethylformamide into a three-neck flask provided with a stirrer and a thermometer, stirring and reacting for 30-50 min under the conditions of 25-30 ℃ and stirring speed of 500-600 r/min, heating to 115-120 ℃ and stirring and reacting for 2-3h, cooling the reaction product to room temperature after the reaction is finished, and removing the solvent by rotary evaporation to obtain an intermediate 4;
the reaction principle is as follows:
step A5: adding the intermediate 4, perfluorobutanol, anhydrous potassium carbonate and chloroform into a three-neck flask provided with a stirrer, a thermometer and an air duct, introducing nitrogen for protection, stirring and reacting for 1-2h under the condition of 5-10 ℃ and stirring speed of 500-600 r/min, heating to 85-90 ℃ and continuing stirring and reacting for 15-20h, cooling the reaction product to room temperature after the reaction is finished, centrifuging, washing the precipitate with distilled water for 3-5 times, and then placing in a vacuum drying oven, and drying for 8-10h under the condition of 60-65 ℃ to obtain the reinforcing filler.
The reaction principle is as follows:
as a further scheme of the invention: the dosage ratio of the 2, 6-di-tert-butylphenol, sodium hydroxide, deionized water, toluene and N, N-dimethylacetamide in the step A1 is 0.1mol:0.15mol:5-10mL:5-10mL:50-60mL, wherein the mass fraction of the concentrated hydrochloric acid is 36-38%.
As a further scheme of the invention: the dosage ratio of the intermediate 1, thionyl chloride and N, N-dimethylformamide in the step A2 is 10mmol:25-30mL:0.1-0.5mL.
As a further scheme of the invention: the dosage ratio of the intermediate 2, the N-bromosuccinimide and the N, N-dimethylformamide in the step A3 is 10mmol:25-30mmol:50-60mL.
As a further scheme of the invention: the dosage ratio of the intermediate 3, the composite particles, the triethylamine and the N, N-dimethylformamide in the step A4 is 0.2-1.2g:2g:0.05-0.1g:30-40mL.
As a further scheme of the invention: the dosage ratio of the intermediate 4, the perfluorobutanol, the anhydrous potassium carbonate and the chloroform in the step A5 is 1g:0.5-2g:0.4-0.6g:30-40mL.
As a further scheme of the invention: the composite particles are prepared by the following steps:
step B1: adding graphite powder, concentrated sulfuric acid and concentrated nitric acid into a three-neck flask with a stirrer and a thermometer, stirring at the temperature of-5-0 ℃ and the stirring rate of 500-600 r/min for reacting for 20-30 min, adding potassium permanganate, continuously stirring for reacting for 2-3h, heating to 35-40 ℃, continuously stirring for reacting for 2-3h, heating to 90-100 ℃ and continuously stirring for reacting for 1-2h, pouring a reaction product into distilled water after the reaction is finished, adding hydrogen peroxide, standing for 10-15h, centrifuging, washing a precipitate with hydrochloric acid solution and distilled water for 3-5 times in sequence, then placing in a vacuum drying oven, and drying at the temperature of 70-80 ℃ for 10-15h to obtain graphene oxide;
step B2: adding graphene oxide, absolute ethyl alcohol and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, performing ultrasonic dispersion for 0.5-1h under the condition of ultrasonic frequency of 35-45kHz, adding ammonia water, then adding tetraethoxysilane solution dropwise while stirring under the condition of temperature of 25-30 ℃ and stirring rate of 500-600 r/min, controlling the dropping rate to be 1-2 drops/s, continuing stirring for reaction for 15-20h after the dropping is finished, centrifuging a reaction product after the reaction is finished, washing a precipitate with distilled water for 3-5 times, then placing in a vacuum drying oven, and drying for 20-25h under the condition of temperature of 60-65 ℃ to obtain composite particles.
As a further scheme of the invention: the dosage ratio of the graphite powder, the concentrated sulfuric acid, the concentrated nitric acid, the potassium permanganate and the hydrogen peroxide in the step B1 is 2g:40-50mL:35-40mL:12g:30-40mL, wherein the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the concentrated nitric acid is 68%, the mass fraction of the hydrogen peroxide is 25%, and the mass fraction of the hydrochloric acid solution is 10%.
As a further scheme of the invention: the dosage ratio of the graphene oxide, the absolute ethyl alcohol, the deionized water, the ammonia water and the tetraethoxysilane solution in the step B2 is 1g:100-120mL:25-30mL:20-25mL:25-30mL, wherein the mass fraction of the ammonia water is 20-25%, and the tetraethoxysilane solution is tetraethoxysilane according to 1g:8-10mL of the solution is dissolved in absolute ethanol.
As a further scheme of the invention: a graphene-containing stretch-resistant polyethylene cable material prepared according to the preparation process of the graphene-containing stretch-resistant polyethylene cable material of any one of claims 1 to 9.
The invention has the beneficial effects that:
according to the graphene-containing stretch-resistant polyethylene cable material and the preparation process thereof, the linear low-density polyethylene, the styrene-butadiene rubber, the reinforcing filler, the polyvinyl alcohol, the zinc stearate and the antioxidant 1010 are added into a mixer, the mixture is uniformly mixed, extruded and granulated in an extruder, and then the granules are dried to obtain the graphene-containing stretch-resistant polyethylene cable material; in the preparation process, the linear low-density polyethylene and the styrene-butadiene rubber are used as main raw materials, and the reinforcing filler is added into the linear low-density polyethylene and the styrene-butadiene rubber, so that the tensile property of the cable material can be greatly improved, the cable can not be easily damaged under the action of external force, and potential safety hazards are avoided;
preparing a reinforcing filler in the process of preparing a graphene-containing stretch-resistant polyethylene cable material, preparing graphene oxide firstly, performing ultrasonic dispersion on the graphene oxide, performing hydrolysis polycondensation reaction on the graphene oxide under an alkaline condition by utilizing tetraethoxysilane, forming nano silicon dioxide by utilizing a sol-gel method, coating the nano silicon dioxide on the surface of the graphene oxide to obtain composite particles, carboxylating 2, 6-di-tert-butylphenol by utilizing carbon dioxide gas as a carboxylating agent, introducing carboxyl to obtain an intermediate 1, performing acyl chlorination on the carboxyl on the intermediate 1 to obtain an intermediate 2, brominating the intermediate 2 by utilizing N-bromosuccinimide, introducing bromine atoms to obtain an intermediate 3, reacting a large number of hydroxyl groups on the surface of the composite particles by utilizing acyl chloride groups on the intermediate 3, connecting chemical bonds of the intermediate 3 to the surface of the composite particles to obtain an intermediate 4, and then reacting bromine atoms on the intermediate 4 with hydroxyl groups on perfluorobutanol to introduce a large number of C-F bonds to obtain the reinforcing filler; the inner core part of the reinforcing filler is graphene oxide, the graphene oxide has good mechanical properties, so that the cable material can be endowed with good mechanical properties, the compatibility between the graphene oxide and a cable material matrix can be improved after the nano silicon dioxide is coated, the mechanical properties of the cable material are further improved, the nano silicon dioxide has good insulativity, the conductivity of the graphene can be effectively reduced, the phenomenon of electric leakage caused by the decrease of the insulativity of the cable material is avoided, the 2, 6-di-tert-butylphenol structure contained on the molecular structure of the reinforcing filler is endowed with good oxidation resistance, the dispersibility of the reinforcing filler can be further improved by the introduced long carbon chain, the occurrence probability of agglomeration is further reduced, the cable material can be endowed with good flexibility, and the introduced C-F bond can be endowed with good stability.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, 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.
Example 1:
the embodiment is a preparation process of a reinforcing filler, comprising the following steps:
step 1: adding 2g of graphite powder, 40mL of 98% by mass concentrated sulfuric acid and 35mL of 68% by mass concentrated nitric acid into a three-neck flask with a stirrer and a thermometer, stirring for 20 min at a temperature of-5 ℃ and a stirring rate of 500 r/min, adding 12g of potassium permanganate, continuing stirring for reaction for 2h, heating to 35 ℃ and continuing stirring for reaction for 1h, heating to 90 ℃, continuing stirring for reaction for 30 h, pouring the reaction product into distilled water after the reaction is finished, adding 30mL of 25% by mass hydrogen peroxide, standing for 10h, centrifuging, washing the precipitate for 3 times sequentially with 10% by mass hydrochloric acid solution and distilled water, then placing in a vacuum drying box, and drying for 10h at a temperature of 70 ℃ to obtain graphene oxide;
step 2: 1g of graphene oxide, 100mL of absolute ethyl alcohol and 25mL of deionized water are added into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, ultrasonic dispersion is carried out for 0.5h under the condition of ultrasonic frequency of 35kHz, then 20mL of ammonia water with mass fraction of 20% is added, and then 25mL of tetraethoxysilane is added dropwise while stirring under the condition of temperature of 25 ℃ and stirring speed of 500 r/min according to 1g:8mL of tetraethoxysilane solution formed by dissolving the tetraethoxysilane into absolute ethyl alcohol, controlling the dropping speed to be 1 drop/s, continuously stirring for reaction for 15h after the dropping, centrifuging a reaction product after the reaction is finished, washing a precipitate with distilled water for 3 times, and then placing the precipitate in a vacuum drying oven, and drying for 20h at the temperature of 60 ℃ to obtain composite particles;
step 3: adding 0.1mL of 2, 6-di-tert-butylphenol, 0.15 mL of sodium hydroxide, 5mL of deionized water, 5mL of toluene and 50mL of LN, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring at a temperature of 25 ℃ and a stirring rate of 500 r/min for reaction of 20 min, heating to reflux, continuing stirring for reaction until no water is separated out, introducing carbon dioxide gas at a temperature of 100 ℃ and a pressure of 0.65MPa until the reaction system does not absorb carbon dioxide gas any more, cooling the reaction product to room temperature after the reaction is finished, adding into distilled water, adjusting the pH to 1 with 36% by mass of concentrated hydrochloric acid, precipitating precipitate, vacuum-filtering, washing a filter cake with distilled water for 3 times, placing in a vacuum drying box, and drying at a temperature of 70 ℃ for 2h to obtain an intermediate 1;
step 4: adding 10mmol of intermediate 1, 25mL of thionyl chloride and 0.1mL of N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring at a temperature of 25 ℃ and a stirring rate of 500 r/min for reaction for 5 min, heating to reflux, continuing stirring for reaction for 5h, cooling the reaction product to room temperature after the reaction is finished, and removing redundant thionyl chloride by rotary evaporation to obtain an intermediate 2;
step 5: adding 10mmo l of intermediate 2, 25mmo l of N-bromosuccinimide and 50mLN, N-dimethylformamide into a three-neck flask with a stirrer and a thermometer, stirring at the temperature of-5 ℃ and the stirring rate of 500 r/min for reaction for 1h, heating to 35 ℃ for continuous stirring for reaction for 10h, adding the reaction product into distilled water after the reaction is finished, precipitating and precipitating, vacuum filtering, and recrystallizing a filter cake with acetone to obtain an intermediate 3;
step 6: adding 0.2g of intermediate 3, 2g of composite particles, 0.05g of triethylamine and 30mLN, N-dimethylformamide into a three-neck flask provided with a stirrer and a thermometer, stirring for 30 min at a temperature of 25 ℃ and a stirring rate of 500 r/min, heating to 115 ℃ and stirring for 2h, cooling the reaction product to room temperature after the reaction is finished, and removing the solvent by rotary evaporation to obtain an intermediate 4;
step 7: 1g of intermediate 4, 0.5g of perfluorobutanol, 0.4g of anhydrous potassium carbonate and 30mL of chloroform are added into a three-neck flask provided with a stirrer, a thermometer and an air duct, nitrogen is introduced for protection, stirring is carried out for reaction for 1h under the condition that the temperature is 5 ℃ and the stirring rate is 500 r/min, then stirring is continued for reaction for 15h under the condition that the temperature is raised to 85 ℃, after the reaction is finished, the reaction product is cooled to room temperature, and then centrifuged, the precipitate is washed with distilled water for 3 times, and then placed in a vacuum drying oven for drying for 8h under the condition that the temperature is 60 ℃, thus obtaining the reinforcing filler.
Example 2:
the embodiment is a preparation process of a reinforcing filler, comprising the following steps:
step 1: adding 2g of graphite powder, 50mL of 98% by mass concentrated sulfuric acid and 40mL of 68% by mass concentrated nitric acid into a three-neck flask with a stirrer and a thermometer, stirring for 30 min at a temperature of 0 ℃ and a stirring rate of 600 r/min, adding 12g of potassium permanganate, continuing stirring for reaction for 3h, heating to 40 ℃ and continuing stirring for reaction for 2h, heating to 100 ℃, pouring the reaction product into distilled water after the reaction is finished, adding 40mL of 25% by mass hydrogen peroxide, standing for 15h, centrifuging, washing the precipitate with 10% by mass hydrochloric acid solution and distilled water for 5 times, placing in a vacuum drying box, and drying for 15h at a temperature of 80 ℃ to obtain graphene oxide;
step 2: 1g of graphene oxide, 120mL of absolute ethyl alcohol and 30mL of deionized water are added into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, ultrasonic dispersion is carried out for 1h under the condition that ultrasonic frequency is 45kHz, then 25mL of ammonia water with mass fraction of 25% is added, and then 30mL of tetraethoxysilane is added dropwise while stirring under the condition that the temperature is 30 ℃ and the stirring rate is 600 r/min according to 1g:10mL of tetraethoxysilane solution formed by dissolving absolute ethyl alcohol is controlled to have the dropping speed of 2 drops/s, stirring reaction is continued for 20 hours after the dropping is finished, the reaction product is centrifuged after the reaction is finished, the precipitate is washed for 5 times by distilled water, and then the precipitate is placed in a vacuum drying oven and dried for 25 hours at the temperature of 65 ℃ to obtain composite particles;
step 3: adding 0.1mL of 2, 6-di-tert-butylphenol, 0.15 mL of sodium hydroxide, 10mL of deionized water, 10mL of toluene and 60mL of LN, N-dimethylacetamide into a three-neck flask provided with a stirrer, a thermometer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring for reaction for 30 min under the condition of 30 ℃ and stirring rate of 600 r/min, heating to reflux, continuing stirring for reaction until no water is separated out, introducing carbon dioxide gas under the condition of 110 ℃ and pressure of 0.7MPa until the reaction system does not absorb carbon dioxide gas, cooling the reaction product to room temperature after the reaction is finished, adding into distilled water, adjusting the pH to 2 with concentrated hydrochloric acid with mass fraction of 38%, precipitating, vacuum-filtering, washing a filter cake with distilled water for 5 times, placing in a vacuum drying box, and drying for 3h under the condition of 75 ℃ to obtain an intermediate 1;
step 4: adding 10mmol of intermediate 1, 30mL of thionyl chloride and 0.5mLN, N-dimethylformamide into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring at a temperature of 30 ℃ and a stirring rate of 600 r/min for reaction for 10 min, heating to reflux, continuing stirring for reaction for 6h, cooling the reaction product to room temperature after the reaction is finished, and removing redundant thionyl chloride by rotary evaporation to obtain an intermediate 2;
step 5: adding 10mmo l of intermediate 2, 30mmo l of N-bromosuccinimide and 60mLN, N-dimethylformamide into a three-neck flask with a stirrer and a thermometer, stirring at the temperature of 0 ℃ and the stirring rate of 600 r/min for reaction for 1.5h, heating to 40 ℃ for continuous stirring for reaction for 15h, adding the reaction product into distilled water after the reaction is finished, precipitating and precipitating, vacuum filtering, and recrystallizing a filter cake with acetone to obtain an intermediate 3;
step 6: 1.2g of an intermediate 3, 2g of composite particles, 0.1g of triethylamine and 40mLN, N-dimethylformamide are added into a three-necked flask provided with a stirrer and a thermometer, 50 min of the mixture is stirred under the condition that the temperature is 30 ℃ and the stirring rate is 600 r/min, then the mixture is heated to 120 ℃ and stirred for 3 hours for reaction, after the reaction is finished, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, so that an intermediate 4 is obtained;
step 7: 1g of intermediate 4, 2g of perfluorobutanol, 0.6g of anhydrous potassium carbonate and 40mL of chloroform are added into a three-neck flask provided with a stirrer, a thermometer and an air duct, nitrogen is introduced for protection, stirring is carried out for 2 hours under the condition that the temperature is 10 ℃ and the stirring rate is 600 r/min, then stirring is continued for 20 hours under the condition that the temperature is raised to 90 ℃, after the reaction is finished, the reaction product is cooled to room temperature, centrifuged, the precipitate is washed 5 times by distilled water, and then placed in a vacuum drying oven, and dried for 8-10 hours under the condition that the temperature is 65 ℃ to obtain the reinforcing filler.
Example 3:
the embodiment is a preparation process of a graphene-containing stretch-resistant polyethylene cable material, which comprises the following steps:
step one: preparing a reinforcing filler for later use according to the preparation process in example 1;
step two: 15 parts of linear low-density polyethylene, 5 parts of styrene-butadiene rubber, 2 parts of reinforcing filler, 7 parts of polyvinyl alcohol, 0.8 part of zinc stearate and 0.4 part of antioxidant 1010 are weighed according to parts by weight for standby;
step three: adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying the granules to obtain the graphene-containing stretch-resistant polyethylene cable material.
Example 4:
the embodiment is a preparation process of a graphene-containing stretch-resistant polyethylene cable material, which comprises the following steps:
step one: preparing a reinforcing filler for later use according to the preparation process in example 2;
step two: weighing 20 parts of linear low-density polyethylene, 9 parts of styrene-butadiene rubber, 12 parts of reinforcing filler, 13 parts of polyvinyl alcohol, 1.4 parts of zinc stearate and 0.6 part of antioxidant for standby;
step three: adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying the granules to obtain the graphene-containing stretch-resistant polyethylene cable material.
Comparative example 1:
comparative example 1 differs from example 4 in that no reinforcing filler was added.
Comparative example 2:
comparative example 2 differs from example 4 in that graphene oxide in step 1 was used instead of the reinforcing filler.
Comparative example 3:
comparative example 3 is a stretch-proof polyethylene cable sheathing compound of example application number CN201410595638.4 and a method of making the same.
The properties of examples 3 to 4 and comparative examples 1 to 3 were examined, and the results are shown in the following table:
| sample of | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Tensile strength, MPa | 35.8 | 37.5 | 23.4 | 31.2 | 25.2 |
| Elongation at break% | 821 | 854 | 462 | 675 | 380 |
Referring to the above table data, according to the comparison of examples 3-4 and comparative examples 1-2, it can be known that the tensile properties of the cable material can be obviously enhanced by adding graphene oxide and the reinforcing filler, and the enhancement effect of the reinforcing filler is more obvious, and according to the comparison of examples 3-4 and comparative example 3, the tensile properties of the cable material of the present invention are obviously higher than those of the cable sheath material in the prior art.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (9)
1. The preparation process of the graphene-containing stretch-resistant polyethylene cable material is characterized by comprising the following steps of:
step one: 15-20 parts of linear low-density polyethylene, 5-9 parts of styrene-butadiene rubber, 2-12 parts of reinforcing filler, 7-13 parts of polyvinyl alcohol, 0.8-1.4 parts of zinc stearate and 0.4-0.6 part of antioxidant are weighed according to parts by weight for standby;
step two: adding linear low-density polyethylene, styrene-butadiene rubber, reinforcing filler, polyvinyl alcohol, zinc stearate and antioxidant 1010 into a mixer, uniformly mixing, extruding and granulating in an extruder, and drying the granules to obtain the graphene-containing stretch-resistant polyethylene cable material;
wherein, the reinforcing filler is prepared by the following steps:
step A1: adding 2, 6-di-tert-butylphenol, sodium hydroxide, deionized water, toluene and N, N-dimethylacetamide into a three-neck flask, stirring and reacting until no water exists, then introducing carbon dioxide gas, continuing stirring and reacting, cooling a reaction product after the reaction is finished, then adding the reaction product into distilled water, adjusting pH, precipitating, vacuum-filtering, washing and drying a filter cake to obtain an intermediate 1;
step A2: adding the intermediate 1, thionyl chloride and N, N-dimethylformamide into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, and then rotationally evaporating to obtain an intermediate 2;
step A3: adding the intermediate 2, N-bromosuccinimide and N, N-dimethylformamide into a three-neck flask, stirring for reaction, adding a reaction product into distilled water after the reaction is finished, precipitating a precipitate, then carrying out vacuum suction filtration, and recrystallizing a filter cake to obtain an intermediate 3;
step A4: adding the intermediate 3, composite particles, triethylamine and N, N-dimethylformamide into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, and then rotationally evaporating to obtain an intermediate 4;
step A5: adding the intermediate 4, perfluorobutanol, anhydrous potassium carbonate and chloroform into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, centrifuging, washing and drying a precipitate to obtain a reinforcing filler;
the composite particles are prepared by the following steps:
step B1: adding graphite powder, concentrated sulfuric acid and concentrated nitric acid into a three-neck flask, stirring for reaction, adding potassium permanganate, continuously stirring for reaction, pouring a reaction product into distilled water after the reaction is finished, adding hydrogen peroxide, standing, centrifuging, washing and drying a precipitate to obtain graphene oxide;
step B2: adding graphene oxide, absolute ethyl alcohol and deionized water into a three-neck flask for ultrasonic dispersion, adding ammonia water, dropwise adding an ethyl orthosilicate solution while stirring, continuing stirring for reaction after the dropwise addition, centrifuging a reaction product after the reaction is finished, washing and drying a precipitate, and obtaining composite particles.
2. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of 2, 6-di-tert-butylphenol, sodium hydroxide, deionized water, toluene and N, N-dimethylacetamide in step A1 is 0.1mol:0.15mol:5-10mL:5-10mL:50-60mL.
3. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the intermediate 1, thionyl chloride and N, N-dimethylformamide in the step A2 is 10mmol:25-30mL:0.1-0.5mL.
4. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the intermediate 2, N-bromosuccinimide and N, N-dimethylformamide in the step A3 is 10mmol:25-30mmol:50-60mL.
5. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the intermediate 3, the composite particles, the triethylamine and the N, N-dimethylformamide in the step A4 is 0.2-1.2g:2g:0.05-0.1g:30-40mL.
6. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the intermediate 4, perfluorobutanol, anhydrous potassium carbonate and chloroform in the step A5 is 1g:0.5-2g:0.4-0.6g:30-40mL.
7. The preparation process of the graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the graphite powder to the concentrated sulfuric acid to the concentrated nitric acid to the potassium permanganate to the hydrogen peroxide in the step B1 is 2g:40-50mL:35-40mL:12g:30-40mL, wherein the mass fraction of the concentrated sulfuric acid is 98%, the mass fraction of the concentrated nitric acid is 68%, and the mass fraction of the hydrogen peroxide is 25%.
8. The process for preparing a graphene-containing stretch-resistant polyethylene cable material according to claim 1, wherein the dosage ratio of the graphene oxide, absolute ethyl alcohol, deionized water, ammonia water and tetraethoxysilane solution in the step B2 is 1g:100-120mL:25-30mL:20-25mL:25-30mL, wherein the mass fraction of the ammonia water is 20-25%, and the tetraethoxysilane solution is tetraethoxysilane according to 1g:8-10mL of the solution is dissolved in absolute ethanol.
9. The graphene-containing stretch-resistant polyethylene cable material is characterized in that the graphene-containing stretch-resistant polyethylene cable material is prepared according to the preparation process of the graphene-containing stretch-resistant polyethylene cable material described in any one of claims 1-8.
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