CN117004111A - Halogen-free flame-retardant cable material for aluminum alloy cable and preparation method thereof - Google Patents
Halogen-free flame-retardant cable material for aluminum alloy cable and preparation method thereof Download PDFInfo
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- CN117004111A CN117004111A CN202310867805.5A CN202310867805A CN117004111A CN 117004111 A CN117004111 A CN 117004111A CN 202310867805 A CN202310867805 A CN 202310867805A CN 117004111 A CN117004111 A CN 117004111A
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- flame retardant
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 73
- 239000000463 material Substances 0.000 title claims abstract description 72
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920013716 polyethylene resin Polymers 0.000 claims abstract description 19
- 229910052582 BN Inorganic materials 0.000 claims abstract description 14
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 14
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 claims abstract description 12
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 80
- 238000006243 chemical reaction Methods 0.000 claims description 52
- 239000007795 chemical reaction product Substances 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 27
- 229920000642 polymer Polymers 0.000 claims description 25
- 239000012065 filter cake Substances 0.000 claims description 23
- 238000001914 filtration Methods 0.000 claims description 23
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- DWSWCPPGLRSPIT-UHFFFAOYSA-N benzo[c][2,1]benzoxaphosphinin-6-ium 6-oxide Chemical compound C1=CC=C2[P+](=O)OC3=CC=CC=C3C2=C1 DWSWCPPGLRSPIT-UHFFFAOYSA-N 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 235000021355 Stearic acid Nutrition 0.000 claims description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 12
- 239000008117 stearic acid Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 11
- 230000001376 precipitating effect Effects 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000008098 formaldehyde solution Substances 0.000 claims description 8
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 7
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 7
- PHMRPWPDDRGGGF-UHFFFAOYSA-N 2-bromoprop-1-ene Chemical compound CC(Br)=C PHMRPWPDDRGGGF-UHFFFAOYSA-N 0.000 claims description 7
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 7
- BXRFQSNOROATLV-UHFFFAOYSA-N 4-nitrobenzaldehyde Chemical compound [O-][N+](=O)C1=CC=C(C=O)C=C1 BXRFQSNOROATLV-UHFFFAOYSA-N 0.000 claims description 7
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 239000001119 stannous chloride Substances 0.000 claims description 7
- 235000011150 stannous chloride Nutrition 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 4
- 239000003208 petroleum Substances 0.000 claims description 4
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052736 halogen Inorganic materials 0.000 abstract description 3
- 150000002367 halogens Chemical class 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 3
- 239000011147 inorganic material Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 36
- 238000010992 reflux Methods 0.000 description 25
- 238000010438 heat treatment Methods 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 18
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 239000004800 polyvinyl chloride Substances 0.000 description 6
- 229920000915 polyvinyl chloride Polymers 0.000 description 6
- 238000007792 addition Methods 0.000 description 3
- 125000003342 alkenyl group Chemical group 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000007259 addition reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical group C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000005821 Claisen rearrangement reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZOXJGFHDIHLPTG-OUBTZVSYSA-N boron-12 Chemical group [12B] ZOXJGFHDIHLPTG-OUBTZVSYSA-N 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000012546 transfer 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
- C08L23/06—Polyethene
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
-
- 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 halogen-free flame-retardant cable material for an aluminum alloy cable and a preparation method thereof, which are used for solving the problems that the flame retardant property of the existing halogen-free cable material is poor, and the mechanical strength of the existing halogen-free cable material is greatly reduced after a large amount of inorganic materials are added; according to the preparation method, the polyethylene resin is used as a main raw material, the heat-resistant performance and the heat resistance performance of the polyethylene resin can be further improved by adding the ethylene propylene diene monomer, the mechanical performance of the polyethylene resin can be further enhanced, the halogen-free high-molecular flame retardant added later can greatly improve the flame retardant performance of the cable material, the cable material does not contain halogen, the mechanical performance and the heat conducting performance of the cable material can be effectively improved by adding the aluminum oxide and the boron nitride later, the heat can be rapidly led out, and the flame retardant performance of the cable material is further improved, so that the halogen-free flame retardant cable material for the aluminum alloy cable is good in flame retardant effect and suitable for being used in a high-temperature environment.
Description
Technical Field
The invention relates to the field of cable materials, in particular to a halogen-free flame-retardant cable material for an aluminum alloy cable and a preparation method thereof.
Background
With the rapid development of the wire and cable industry, the demand of the wire and cable is gradually increased, and the application is more and more extensive, wherein the aluminum alloy cable is a novel material power cable which uses an aluminum alloy material as a conductor and adopts advanced technologies such as a special roll forming molded line stranding production process, annealing treatment and the like, has good mechanical properties and electrical properties, and can be widely applied to various fields of national economy.
With the development of society, wires and cables are increasingly widely applied to various fields, such as transportation, communication, construction and the like, PVC cable materials are prepared by taking polyvinyl chloride as basic resin and adding other auxiliary agents and then adopting extrusion and other methods, and the PVC cable materials contain a large amount of chlorine elements and have excellent flame retardant property, so that the PVC cable materials are main matrix materials of the cable materials, however, a large amount of toxic gases are generated when the PVC burns, and casualties are easily caused. With increasing importance of environmental protection and life safety, how to reduce the occurrence rate of fire and the death rate when the fire occurs, and no halogenation becomes the development direction of the wire and cable industry. At present, PVC materials are not used any more in the production of halogen-free cable materials, but other halogen-free polymers are selected, but the flame retardant property of the cable materials prepared from the existing halogen-free polymers is poor, and the flame retardant effect can be achieved by adding a large amount of magnesium hydroxide or other hydroxides into halogen-free polymer base materials, however, the addition of a large amount of inorganic materials influences the physical and mechanical properties and the processing technological properties of the cable materials.
How to improve the poor flame retardant property of the existing halogen-free cable material, and the great reduction of the mechanical strength of the cable material caused by adding a large amount of inorganic materials is the key of the invention.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a halogen-free flame-retardant cable material for an aluminum alloy cable and a preparation method thereof: the halogen-free flame-retardant cable material for the aluminum alloy cable is prepared by adding polyethylene resin, ethylene propylene diene monomer, a halogen-free high polymer flame retardant, stearic acid, aluminum oxide, boron nitride and a PE-g-MAH compatilizer into an internal mixer for internal mixing to obtain an internal mixing material, adding the internal mixing material into an extruder, and performing extrusion granulation.
The aim of the invention can be achieved by the following technical scheme:
the halogen-free flame-retardant cable material for the aluminum alloy cable comprises the following components in parts by weight:
40-50 parts of polyethylene resin, 20-25 parts of ethylene propylene diene monomer rubber, 15-35 parts of halogen-free high polymer flame retardant, 2-8 parts of stearic acid, 4-6 parts of alumina, 3-7 parts of boron nitride and 3-12 parts of PE-g-MAH compatilizer;
the halogen-free high polymer flame retardant is prepared by the following steps:
step s1: adding bisphenol S, sodium hydroxide, deionized water and toluene into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 15-20 min under the conditions of 25-30 ℃ and stirring speed of 350-400 r/min, then adding 2-bromopropene, heating to 55-60 ℃ and continuing stirring and reacting for 20-30 min, heating to reflux and continuing stirring and reacting for 8-10h, cooling the reaction product to room temperature after the reaction is finished, standing for 10-15h, vacuum filtering, placing the filter cake in a vacuum drying oven, and drying for 2-3h under the conditions of 60-65 ℃ to obtain an intermediate 1;
the reaction principle is as follows:
step s2: adding the intermediate 1,2, 4-trichlorobenzene into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 15-20 min under the condition that the temperature is 25-30 ℃ and the stirring speed is 350-400 r/min, heating to reflux, continuing stirring and reacting for 5-6h, cooling the reaction product to room temperature after the reaction is finished, rotationally evaporating to remove the solvent, adding the solvent into 120# solvent oil, stirring and precipitating, vacuum filtering, placing the filter cake into a vacuum drying oven, and drying for 2-3h under the condition that the temperature is 60-65 ℃ to obtain an intermediate 2;
the reaction principle is as follows:
step s3: adding the intermediate 2, DOPO and N, N-dimethylformamide into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 1-2h under the condition that the temperature is 50-55 ℃ and the stirring speed is 350-400 r/min, heating to reflux, continuing stirring and reacting for 20-30h, cooling the reaction product to room temperature after the reaction is finished, washing for 3-5 times with distilled water, drying with anhydrous sodium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain an intermediate 3;
the reaction principle is as follows:
step s4: adding p-nitrobenzaldehyde, p-phenylenediamine and absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, stirring and reacting for 20-30 min under the conditions of 25-30 ℃ and stirring speed of 350-400 r/min, adding glacial acetic acid, introducing nitrogen for protection, heating to 60-65 ℃ and continuing stirring and reacting for 15-20h, cooling the reaction product to room temperature after the reaction, vacuum filtering, placing a filter cake in a vacuum drying box, and drying for 8-10h under the conditions of 75-80 ℃ to obtain an intermediate 4;
the reaction principle is as follows:
step s5: adding the intermediate 4, DOPO and absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, introducing nitrogen for protection, stirring and reacting for 15-20h under the condition that the temperature is 60-65 ℃ and the stirring speed is 350-400 r/min, cooling the reaction product to room temperature after the reaction is finished, pouring the reaction product into petroleum ether, precipitating, vacuum filtering, washing a filter cake with distilled water for 3-5 times, and then placing the filter cake in a vacuum drying oven, and drying for 8-10h under the condition that the temperature is 75-80 ℃ to obtain an intermediate 5;
the reaction principle is as follows:
step s6: adding the intermediate 5, stannous chloride and absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 35-40 min under the conditions of 25-30 ℃ and stirring speed of 350-400 r/min, heating to reflux, continuing stirring and reacting for 8-10h, cooling the reaction product to room temperature after the reaction is finished, adjusting the pH value to 8-9 by using sodium hydroxide solution, precipitating, vacuum filtering, and recrystallizing a filter cake by using dichloromethane to obtain an intermediate 6;
the reaction principle is as follows:
step s7: adding the intermediate 3, the intermediate 6 and chloroform into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant pressure dropping funnel, introducing nitrogen for protection, stirring and reacting for 15-20 min under the condition that the temperature is-5-0 ℃ and the stirring rate is 350-400 r/min, then adding formaldehyde solution dropwise while stirring, controlling the dropping rate to be 1-2 drops/s, heating to 60-65 ℃ after the dropping, continuing stirring and reacting for 20-30h, cooling the reaction product to room temperature after the reaction is finished, washing for 3-5 times with distilled water, standing for layering, drying the organic phase with anhydrous sodium sulfate, vacuum suction filtering, and removing the solvent by rotary evaporation of filtrate to obtain the halogen-free high polymer flame retardant.
The reaction principle is as follows:
as a further scheme of the invention: the bisphenol S, sodium hydroxide, deionized water, toluene and 2-bromopropene in step S1 were used in an amount ratio of 0.1mol:3-5g:20-30mL:30-35mL:0.25-0.3mol.
As a further scheme of the invention: the ratio of the amount of the intermediate 1,2, 4-trichlorobenzene used in step s2 was 10g:50-60mL.
As a further scheme of the invention: the ratio of the amounts of intermediate 2, DOPO and N, N-dimethylformamide used in step s3 was 10mmol:22-25mmol:50-60mL.
As a further scheme of the invention: the dosage ratio of the p-nitrobenzaldehyde, the p-phenylenediamine, the absolute ethyl alcohol and the glacial acetic acid in the step s4 is 20mmo l:10mmol:30-40mL:0.5-1mL.
As a further scheme of the invention: the dosage ratio of the intermediate 4, DOPO and absolute ethanol in the step s5 is 10mmol:22-25mmol:70-80mL.
As a further scheme of the invention: the use amount ratio of the intermediate 5, stannous chloride and absolute ethyl alcohol in the step s6 is 10mmol:0.1-0.11mol:100-120mL, wherein the mass fraction of the sodium hydroxide solution is 20-25%.
As a further scheme of the invention: the ratio of the amount of the intermediate 3, the intermediate 6, chloroform and formaldehyde solution in the step s7 is 10mmol:10mmol:100-120mL:10-15mL, wherein the mass fraction of the formaldehyde solution is 37%.
As a further scheme of the invention: the preparation method of the halogen-free flame-retardant cable material for the aluminum alloy cable comprises the following steps:
step one: weighing 40-50 parts of polyethylene resin, 20-25 parts of ethylene propylene diene monomer, 15-35 parts of halogen-free high polymer flame retardant, 2-8 parts of stearic acid, 4-6 parts of aluminum oxide, 3-7 parts of boron nitride and 3-12 parts of PE-g-MAH compatilizer according to parts by weight for standby;
step two: adding polyethylene resin, ethylene propylene diene monomer, halogen-free high polymer flame retardant, stearic acid, alumina, boron nitride and PE-g-MAH compatilizer into an internal mixer, and banburying for 30-50min at 140-160 ℃ to obtain banburying materials;
step three: adding the banburying material into an extruder, and performing extrusion granulation to obtain the halogen-free flame-retardant cable material for the aluminum alloy cable.
The invention has the beneficial effects that:
according to the halogen-free flame-retardant cable material for the aluminum alloy cable and the preparation method thereof, polyethylene resin, ethylene propylene diene monomer, a halogen-free high polymer flame retardant, stearic acid, aluminum oxide, boron nitride and a PE-g-MAH compatilizer are added into an internal mixer for banburying to obtain a banburying material, the banburying material is added into an extruder, and extrusion granulation is carried out to obtain the halogen-free flame-retardant cable material for the aluminum alloy cable; the preparation method takes the polyethylene resin as a main raw material, the polyethylene resin is a very common cable material, has good insulating property, can effectively isolate current in the cable, avoids the problems of current leakage, short circuit and the like, has good heat resistance, can keep stable performance under high-temperature environment, can further improve the heat resistance of the polyethylene resin by adding the ethylene propylene diene monomer rubber, can further enhance the mechanical property of the polyethylene resin, can greatly improve the flame resistance of the cable material by adding the halogen-free high-molecular flame retardant, does not contain halogen, avoids harmful gas generated by the traditional halogen-containing flame retardant, has the advantages of environmental protection and health, can effectively improve the mechanical property and the heat conductivity of the cable material by adding the aluminum oxide and the boron nitride, can quickly conduct out heat, and further improves the flame resistance of the cable material, so that the halogen-free flame-retardant cable material for the aluminum alloy cable has good flame resistance effect, can be suitable for being used under the high-temperature environment, and widens the application range of the halogen-free flame-retardant cable material for the aluminum alloy cable;
firstly, utilizing hydroxyl on bisphenol S to react with bromine atoms on 2-bromopropene to introduce alkenyl to generate an intermediate 1, then refluxing the intermediate 1 in 1,2, 4-trichlorobenzene at 220 ℃, generating a claisen rearrangement reaction at the moment, transferring alkenyl to hydroxyl ortho-position to obtain an intermediate 2, then generating an addition reaction between alkenyl on the intermediate 2 and P-H bond on DOPO to obtain an intermediate 3, utilizing aldehyde group on P-nitrobenzaldehyde to react with amino on P-phenylenediamine to form C=N bond to obtain an intermediate 4, then generating an addition reaction between C=N bond on the intermediate 4 and P-H bond on DOPO to obtain an intermediate 5, then reducing nitro on the intermediate 5 to amino under the action of stannous chloride to obtain an intermediate 6, and then generating reaction between the intermediate 3, the intermediate 6 and formaldehyde to form a benzoxazine structure to obtain the halogen-free high-molecular flame retardant; the halogen-free high-molecular flame retardant is an organic substance, has good compatibility with polyethylene, can not cause adverse effect on mechanical properties of the polyethylene, and can be enhanced, and the halogen-free high-molecular flame retardant contains a large number of annular structures on molecules to endow the halogen-free high-molecular flame retardant with good thermal stability, and contains a large number of organic phosphorus and organic nitrogen on the molecules, so that the organic phosphorus can catalyze the organic substance to dehydrate to form carbon during combustion to form a carbon deposit layer, can prevent heat transfer and oxygen diffusion, and can generate a large number of nonflammable gases during combustion to play a role in diluting and even isolating the flammable gases, thereby effectively preventing flame propagation and realizing the aim of flame retardance.
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 method of a halogen-free high polymer flame retardant, which comprises the following steps:
step s1: adding 0.1mol of bisphenol S, 3g of sodium hydroxide, 20mL of deionized water and 30mL of toluene into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 15 min under the condition that the temperature is 25 ℃ and the stirring rate is 350 r/min, adding 0.25 mol of 2-bromopropene and heating to 55 ℃ for continuously stirring and reacting for 20 min, heating to reflux for continuously stirring and reacting for 8h, cooling the reaction product to room temperature after the reaction is finished, standing for 10-15h, vacuum filtering, placing a filter cake in a vacuum drying oven, and drying for 2h under the condition that the temperature is 60 ℃ to obtain an intermediate 1;
step s2: 10g of intermediate 1, 50ml of 1,2, 4-trichlorobenzene is added into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, nitrogen is introduced for protection, stirring is carried out for reaction for 15 min under the condition that the temperature is 25 ℃ and the stirring rate is 350 r/min, then the reaction is continued under the condition that the temperature is raised to reflux for 5h, the reaction product is cooled to room temperature after the reaction is finished, the solvent is removed by rotary evaporation, then the reaction product is added into 120# solvent oil for stirring and precipitation, then vacuum filtration is carried out, a filter cake is placed into a vacuum drying box, and the reaction product is dried for 2h under the condition that the temperature is 60 ℃ to obtain intermediate 2;
step s3: adding 10mmol of intermediate 2, 22 mmol of DOPO and 50 mmon of N-dimethylformamide into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 1h under the condition that the temperature is 50 ℃ and the stirring speed is 350 r/min, heating to reflux, continuing stirring and reacting for 20h, cooling the reaction product to room temperature after the reaction is finished, washing with distilled water for 3 times, drying with anhydrous sodium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain an intermediate 3;
step s4: adding 20mmol of p-nitrobenzaldehyde, 10mmol of p-phenylenediamine and 30mL of absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, stirring at a temperature of 25 ℃ and a stirring rate of 350 r/min for reacting for 20 min, adding 0.5mL of glacial acetic acid, introducing nitrogen for protection, heating to 60 ℃ for continuously stirring for reacting for 15h, cooling a reaction product to room temperature after the reaction is finished, vacuum filtering, placing a filter cake into a vacuum drying oven, and drying at a temperature of 75 ℃ for 8h to obtain an intermediate 4;
step s5: adding 10mmol of intermediate 4, 22 mmol of DOPO and 70mL of absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, introducing nitrogen for protection, stirring and reacting for 15h under the condition that the temperature is 60 ℃ and the stirring rate is 350 r/min, cooling the reaction product to room temperature after the reaction is finished, pouring the reaction product into petroleum ether, precipitating, vacuum filtering, washing a filter cake with distilled water for 3 times, and then placing the filter cake in a vacuum drying oven, and drying for 8h under the condition that the temperature is 75 ℃ to obtain an intermediate 5;
step s6: adding 10mmol of intermediate 5, 0.1 mole of stannous chloride and 100mL of absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 35 min under the condition that the temperature is 25 ℃ and the stirring speed is 350 r/min, heating to reflux, continuing stirring and reacting for 8h, cooling a reaction product to room temperature after the reaction is finished, adjusting the pH value to 8 by using a sodium hydroxide solution with the mass fraction of 20%, precipitating a precipitate, vacuum filtering, and recrystallizing a filter cake by using dichloromethane to obtain an intermediate 6;
step s7: adding 10mmol intermediate 3, 10mmol intermediate 6 and 100mL of chloroform into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant pressure dropping funnel, introducing nitrogen for protection, stirring and reacting for 15 min under the condition that the temperature is minus 5 ℃ and the stirring rate is 350 r/min, then adding 10mL of formaldehyde solution with the mass fraction of 37% dropwise while stirring, controlling the dropping rate to be 1 drop/s, continuously stirring and reacting for 20h under the condition that the temperature is raised to 60 ℃ after the dropping, cooling the reaction product to room temperature after the reaction is finished, washing for 3 times by distilled water, standing for layering, drying an organic phase by using anhydrous sodium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain the halogen-free high polymer flame retardant.
Example 2:
the embodiment is a preparation method of a halogen-free high polymer flame retardant, which comprises the following steps:
step s1: adding 0.1mol of bisphenol S, 5g of sodium hydroxide, 30mL of deionized water and 35mL of toluene into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring and reacting for 20 min under the condition that the temperature is 30 ℃ and the stirring rate is 400 r/min, adding 0.3mol of 2-bromopropene and heating to 60 ℃ for continuous stirring and reacting for 30 min, heating to reflux for continuous stirring and reacting for 10h, cooling the reaction product to room temperature after the reaction is finished, standing for 15h, vacuum filtering, and placing a filter cake in a vacuum drying oven for 3h under the condition that the temperature is 65 ℃ to obtain an intermediate 1;
step s2: adding 10g of intermediate 1, 60ml of 1,2, 4-trichlorobenzene into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring for reaction for 20 min under the condition of 30 ℃ and stirring rate of 400 r/min, heating to reflux, continuing stirring for reaction for 6h, cooling the reaction product to room temperature after the reaction is finished, removing the solvent by rotary evaporation, adding the solvent into 120# solvent oil, stirring for precipitation, vacuum filtering, placing a filter cake into a vacuum drying box, and drying for 3h under the condition of 65 ℃ to obtain an intermediate 2;
step s3: adding 10mmo l of intermediate 2, 25mmo l of DOPO and 60mLN, N-dimethylformamide into a three-neck flask provided with a thermometer, a stirrer, an air duct and a reflux condenser, introducing nitrogen for protection, stirring at a temperature of 55 ℃ and a stirring rate of 400 r/min for reaction for 2 hours, heating to reflux, continuing stirring for reaction for 30 hours, cooling the reaction product to room temperature after the reaction is finished, washing with distilled water for 5 times, drying with anhydrous sodium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain an intermediate 3;
step s4: adding 20mmol of p-nitrobenzaldehyde, 10mmol of p-phenylenediamine and 40mL of absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, stirring and reacting for 30 min under the condition that the temperature is 30 ℃ and the stirring speed is 400 r/min, adding 1mL of glacial acetic acid, introducing nitrogen for protection, heating to 65 ℃ and continuing stirring and reacting for 20h, cooling the reaction product to room temperature after the reaction is finished, vacuum filtering, placing a filter cake into a vacuum drying box, and drying for 10h under the condition that the temperature is 80 ℃ to obtain an intermediate 4;
step s5: adding 10mmol of intermediate 4, 25mmol of DOPO and 80mL of absolute ethyl alcohol into a three-neck flask provided with a thermometer, a stirrer and an air duct, introducing nitrogen for protection, stirring and reacting for 20h under the condition that the temperature is 65 ℃ and the stirring rate is 400 r/min, cooling the reaction product to room temperature after the reaction is finished, pouring the reaction product into petroleum ether, precipitating, vacuum filtering, washing a filter cake with distilled water for 5 times, and then placing the filter cake in a vacuum drying oven, and drying for 10h under the condition that the temperature is 80 ℃ to obtain an intermediate 5;
step s6: adding 10mmol of intermediate 5, 0.11 mole of stannous chloride and 120mL of absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 40 min under the condition that the temperature is 30 ℃ and the stirring rate is 400 r/min, heating to reflux, continuing stirring and reacting for 10h, cooling a reaction product to room temperature after the reaction is finished, adjusting the pH value to 9 by using a sodium hydroxide solution with the mass fraction of 25%, precipitating a precipitate, vacuum filtering, and recrystallizing a filter cake by using dichloromethane to obtain an intermediate 6;
step s7: adding 10mmol intermediate 3, 10mmol intermediate 6 and 120mL of chloroform into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant pressure dropping funnel, introducing nitrogen for protection, stirring and reacting for 20 min under the condition that the temperature is 0 ℃ and the stirring rate is 400 r/min, then adding 15mL of formaldehyde solution with the mass fraction of 37% dropwise while stirring, controlling the dropping rate to be 2 drops/s, continuously stirring and reacting for 30h under the condition that the temperature is raised to 65 ℃ after the dropping is finished, cooling the reaction product to room temperature after the reaction is finished, washing for 5 times by distilled water, standing for layering, drying an organic phase by using anhydrous sodium sulfate, vacuum filtering, and rotationally evaporating the filtrate to remove the solvent to obtain the halogen-free high polymer flame retardant.
Example 3:
the embodiment is a preparation method of a halogen-free flame-retardant cable material for an aluminum alloy cable, which comprises the following steps:
step one: weighing 40 parts of polyethylene resin, 20 parts of ethylene propylene diene monomer, 15 parts of halogen-free high polymer flame retardant from example 1,2 parts of stearic acid, 4 parts of aluminum oxide, 3 parts of boron nitride and 3 parts of PE-g-MAH compatilizer for later use;
step two: adding polyethylene resin, ethylene propylene diene monomer, a halogen-free high polymer flame retardant, stearic acid, aluminum oxide, boron nitride and a PE-g-MAH compatilizer into an internal mixer, and banburying for 30 min at the temperature of 140 ℃ to obtain a banburying material;
step three: adding the banburying material into an extruder, and performing extrusion granulation to obtain the halogen-free flame-retardant cable material for the aluminum alloy cable.
Example 4:
the embodiment is a preparation method of a halogen-free flame-retardant cable material for an aluminum alloy cable, which comprises the following steps:
step one: weighing 50 parts of polyethylene resin, 25 parts of ethylene propylene diene monomer, 35 parts of halogen-free high polymer flame retardant from example 2, 8 parts of stearic acid, 6 parts of aluminum oxide, 7 parts of boron nitride and 12 parts of PE-g-MAH compatilizer for later use;
step two: adding polyethylene resin, ethylene propylene diene monomer, halogen-free high polymer flame retardant, stearic acid, alumina, boron nitride and PE-g-MAH compatilizer into an internal mixer, and banburying for 50min at 160 ℃ to obtain a banburying material;
step three: adding the banburying material into an extruder, and performing extrusion granulation to obtain the halogen-free flame-retardant cable material for the aluminum alloy cable.
Comparative example 1
This comparative example differs from example 4 in that no halogen-free polymeric flame retardant was added.
Comparative example 2
This comparative example differs from example 4 in that DOPO was added instead of the halogen-free polymeric flame retardant.
Comparative example 3
The comparative example is a cable material prepared by the method of example 1 of a halogen-free flame-retardant low-density cable material for aluminum alloy cables according to the application number of CN 201911131347.9.
The properties of the halogen-free flame retardant cable materials for aluminum alloy cables of examples 3 to 4 and comparative examples 1 to 3 were tested, and the test results are shown in the following table:
referring to the data in the table, according to the comparison between the examples 3-4 and the comparative examples 1-3, it can be known that the addition of DOPO and the halogen-free polymer flame retardant can greatly improve the flame retardant property of the halogen-free flame retardant cable material for the aluminum alloy cable, the improvement effect of the halogen-free polymer flame retardant is more obvious, and the tensile strength of the halogen-free flame retardant cable material for the aluminum alloy cable is excellent, which indicates that the mechanical property of the halogen-free flame retardant cable material for the aluminum alloy cable is good.
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 halogen-free flame-retardant cable material for the aluminum alloy cable is characterized in that XXX comprises the following components in parts by weight:
40-50 parts of polyethylene resin, 20-25 parts of ethylene propylene diene monomer rubber, 15-35 parts of halogen-free high polymer flame retardant, 2-8 parts of stearic acid, 4-6 parts of alumina, 3-7 parts of boron nitride and 3-12 parts of PE-g-MAH compatilizer;
the halogen-free high polymer flame retardant is prepared by the following steps:
step s1: adding bisphenol S, sodium hydroxide, deionized water and toluene into a three-neck flask, stirring for reaction, adding 2-bromopropene, continuing stirring for reaction, cooling a reaction product after the reaction is finished, standing, vacuum filtering, and drying a filter cake to obtain an intermediate 1;
step s2: adding the intermediate 1 and 1,2, 4-trichlorobenzene into a three-neck flask for stirring reaction, cooling a reaction product after the reaction is finished, performing rotary evaporation, adding the reaction product into 120# solvent oil for stirring to separate out precipitate, performing vacuum filtration, and drying a filter cake to obtain an intermediate 2;
step s3: adding the intermediate 2, DOPO and N, N-dimethylformamide into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, washing, drying, vacuum filtering, and rotationally evaporating filtrate to obtain an intermediate 3;
step s4: adding p-nitrobenzaldehyde, p-phenylenediamine and absolute ethyl alcohol into a three-neck flask, stirring for reaction, adding glacial acetic acid, continuing stirring for reaction, cooling a reaction product after the reaction is finished, performing vacuum filtration, and drying a filter cake to obtain an intermediate 4;
step s5: adding the intermediate 4, DOPO and absolute ethyl alcohol into a three-neck flask, stirring for reaction, cooling a reaction product after the reaction is finished, pouring the reaction product into petroleum ether, precipitating a precipitate, performing vacuum filtration, washing and drying a filter cake to obtain an intermediate 5;
step s6: adding the intermediate 5, stannous chloride and absolute ethyl alcohol into a three-neck flask for stirring reaction, cooling a reaction product after the reaction is finished, then adjusting pH, precipitating a precipitate, and then carrying out vacuum suction filtration to recrystallize a filter cake to obtain an intermediate 6;
step s7: adding the intermediate 3, the intermediate 6 and chloroform into a three-neck flask, stirring for reaction, dropwise adding formaldehyde solution while stirring, continuing stirring for reaction after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, washing, standing for layering, drying an organic phase, vacuum filtering, and rotationally evaporating filtrate to obtain the halogen-free high polymer flame retardant.
2. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the amount ratio of bisphenol S, sodium hydroxide, deionized water, toluene and 2-bromopropene in step S1 is 0.1mol:3-5g:20-30mL:30-35mL:0.25-0.3mol.
3. A halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the intermediate 1,2, 4-trichlorobenzene in step s2 is used in an amount ratio of 10g:50-60mL.
4. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the ratio of the intermediate 2, DOPO and N, N-dimethylformamide in step s3 is 10mmol:22-25mmol:50-60mL.
5. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the dosage ratio of p-nitrobenzaldehyde, p-phenylenediamine, absolute ethyl alcohol and glacial acetic acid in the step s4 is 20mmol:10mmol:30-40mL:0.5-1mL.
6. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the usage ratio of the intermediate 4, DOPO and absolute ethanol in step s5 is 10mmol:22-25mmol:70-80mL.
7. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the intermediate 5, stannous chloride and absolute ethyl alcohol in the step s6 are used in an amount ratio of 10mmol:0.1 to 0.11mol:100-120mL.
8. The halogen-free flame retardant cable material for aluminum alloy cables according to claim 1, wherein the ratio of the intermediate 3, the intermediate 6, chloroform and formaldehyde solution in the step s7 is 10mmol:10mmol:100-120mL:10-15mL, wherein the mass fraction of the formaldehyde solution is 37%.
9. The preparation method of the halogen-free flame-retardant cable material for the aluminum alloy cable is characterized by comprising the following steps of:
step one: weighing 40-50 parts of polyethylene resin, 20-25 parts of ethylene propylene diene monomer, 15-35 parts of halogen-free high polymer flame retardant, 2-8 parts of stearic acid, 4-6 parts of aluminum oxide, 3-7 parts of boron nitride and 3-12 parts of PE-g-MAH compatilizer according to parts by weight for standby;
step two: adding polyethylene resin, ethylene propylene diene monomer, halogen-free high polymer flame retardant, stearic acid, alumina, boron nitride and PE-g-MAH compatilizer into an internal mixer, and banburying for 30-50min at 140-160 ℃ to obtain banburying materials;
step three: adding the banburying material into an extruder, and performing extrusion granulation to obtain the halogen-free flame-retardant cable material for the aluminum alloy cable.
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