CN119144095A - Flame-retardant high-strength insulating material and preparation process thereof - Google Patents
Flame-retardant high-strength insulating material and preparation process thereof Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 61
- 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 59
- 239000011810 insulating material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 35
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 35
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 35
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 14
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 12
- 229920003020 cross-linked polyethylene Polymers 0.000 claims abstract description 12
- 239000004703 cross-linked polyethylene Substances 0.000 claims abstract description 12
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 12
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 12
- 229920000915 polyvinyl chloride Polymers 0.000 claims abstract description 12
- 239000004800 polyvinyl chloride Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- 238000002156 mixing Methods 0.000 claims description 41
- 229910021389 graphene Inorganic materials 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 28
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 22
- 150000003863 ammonium salts Chemical class 0.000 claims description 20
- 150000001875 compounds Chemical class 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 12
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000010025 steaming Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- ACTRVOBWPAIOHC-UHFFFAOYSA-N succimer Chemical compound OC(=O)C(S)C(S)C(O)=O ACTRVOBWPAIOHC-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical compound COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 claims description 9
- FGQOOHJZONJGDT-UHFFFAOYSA-N vanillin Natural products COC1=CC(O)=CC(C=O)=C1 FGQOOHJZONJGDT-UHFFFAOYSA-N 0.000 claims description 9
- 235000012141 vanillin Nutrition 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- CASUWPDYGGAUQV-UHFFFAOYSA-M potassium;methanol;hydroxide Chemical compound [OH-].[K+].OC CASUWPDYGGAUQV-UHFFFAOYSA-M 0.000 claims description 8
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 claims description 7
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 7
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 7
- FVFVNNKYKYZTJU-UHFFFAOYSA-N 6-chloro-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC(N)=NC(Cl)=N1 FVFVNNKYKYZTJU-UHFFFAOYSA-N 0.000 claims description 7
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 7
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 7
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 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 group 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 description 3
- 229920006225 ethylene-methyl acrylate Polymers 0.000 claims description 3
- 239000005043 ethylene-methyl acrylate Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 229920002285 poly(styrene-co-acrylonitrile) Polymers 0.000 claims description 2
- 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 4
- 239000012774 insulation material Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 20
- 229920001690 polydopamine Polymers 0.000 abstract description 9
- 230000009471 action Effects 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000012744 reinforcing agent Substances 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000034 method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000012650 click reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 description 1
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical group CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229960003638 dopamine Drugs 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005935 nucleophilic addition reaction Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical group 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011593 sulfur Substances 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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
-
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of insulating materials, in particular to a flame-retardant high-strength insulating material and a preparation process thereof. The insulating material comprises, by weight, 50-60 parts of polyvinyl chloride, 20-40 parts of crosslinked polyethylene, 10-15 parts of an ethylene-vinyl acetate copolymer, 20-40 parts of a flame retardant, 5-15 parts of talcum powder, 10-20 parts of calcium carbonate, 6-12 parts of a compatilizer and 3-8 parts of an antioxidant. According to the invention, the flame retardant is prepared by taking ammonium polyphosphate as an acid source, polydopamine as a char forming agent and modified graphene oxide as a reinforcing agent, and the flame retardant is added into a polyvinyl chloride and crosslinked polyethylene insulating material base material, and the combined action of an ethylene-vinyl acetate copolymer, talcum powder, calcium carbonate, a compatilizer and an antioxidant is combined, so that the prepared insulating material has excellent mechanical properties and excellent flame retardant property, and the service life of the material is prolonged.
Description
Technical Field
The invention relates to the technical field of insulating materials, in particular to a flame-retardant high-strength insulating material and a preparation process thereof.
Background
With rapid development of industrialization and modern technology, demands of various high-strength insulating materials in the fields of electric, electronic, aerospace, construction and the like are increasing. These materials are required to have not only excellent insulating properties but also flame retardancy to ensure safety. Therefore, it is important to develop an insulating material having both high strength and excellent flame retardancy.
At present, a plurality of flame retardants are easy to migrate in a high-temperature environment, so that the flame retardant property of the material is weakened along with time, and therefore, lasting safety protection cannot be provided for equipment, and in the process of adding the flame retardants, the mechanical strength of the material is often reduced, so that the requirement on a high-strength insulating material cannot be met. The compatibility difference between the flame retardant and the matrix may further impair the mechanical properties of the material.
Therefore, we propose a flame retardant high strength insulating material and a process for preparing the same.
Disclosure of Invention
The invention aims to provide a flame-retardant high-strength insulating material and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
A preparation process of a flame-retardant high-strength insulating material comprises the following steps:
Step S1, ultrasonically dispersing modified graphene oxide in absolute ethyl alcohol, adding modified ammonium polyphosphate, continuously ultrasonically dispersing for 15-30min, and performing rotary steaming, washing and drying to obtain a flame retardant;
and S2, uniformly mixing polyvinyl chloride, crosslinked polyethylene, ethylene-vinyl acetate copolymer, flame retardant, talcum powder, calcium carbonate, compatilizer and antioxidant to obtain a mixture, and putting the mixture into extrusion equipment for mixing, extruding and granulating to obtain the insulating material.
Further, the insulating material comprises, by weight, 50-60 parts of polyvinyl chloride, 20-40 parts of crosslinked polyethylene, 10-15 parts of an ethylene-vinyl acetate copolymer, 20-40 parts of a flame retardant, 5-15 parts of talcum powder, 10-20 parts of calcium carbonate, 6-12 parts of a compatilizer and 3-8 parts of an antioxidant.
Further, the flame retardant comprises, by weight, 5-10 parts of modified graphene oxide and 15-30 parts of modified ammonium polyphosphate.
Further, in the step S1, the mass ratio of the modified graphene oxide to the absolute ethyl alcohol is 1 (90-110).
Further, the preparation method of the modified graphene oxide comprises the following steps:
Uniformly mixing 2-chloro-4, 6-diamino-1, 3, 5-triazine and absolute ethyl alcohol, dripping 2, 3-dimercaptosuccinic acid and KOH methanol solution, finishing dripping for 20-40min, reacting for 24-28h at 70-80 ℃, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing vanillin, the sulfhydryl-containing compound and absolute ethyl alcohol under the protection of nitrogen, reacting for 8-10h at 65-75 ℃, adding DOPO, continuously reacting for 10-12h, and performing rotary steaming, washing and drying to obtain modified DOPO;
Mixing graphene oxide aqueous solution, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, performing ultrasonic dispersion for 30-60min, adding a mixed solution of oleylamine, ethanol and deionized water, continuing ultrasonic dispersion for 2-3h, stirring for 22-24h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
and (3) uniformly mixing the graphene oxide containing double bonds, the modified DOPO and the photoinitiator, and irradiating with ultraviolet to obtain the modified graphene oxide.
According to the technical scheme, 2-chloro-4, 6-diammine-1, 3, 5-triazine is used as a raw material and reacts with sulfhydryl in 2, 3-dimercaptosuccinic acid under a strong alkali condition to obtain a sulfhydryl-containing compound with a triazine structure and amino groups, vanillin, the sulfhydryl-containing compound and 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) are subjected to nucleophilic addition reaction to obtain modified DOPO with N, S, P elements, then aliphatic long-chain oleylamine is grafted on graphene oxide to obtain graphene oxide with double bonds, compatibility and dispersibility of the graphene oxide with other components are improved, and finally, remaining sulfhydryl in the modified DOPO and the graphene oxide with double bonds are subjected to sulfhydryl-alkene click reaction to obtain the modified graphene oxide with excellent mechanical property and flame retardant property.
Further, in the step (1), the mass ratio of the 2-chloro-4, 6-diammine-1, 3, 5-triazine, the 2, 3-dimercaptosuccinic acid and the absolute ethyl alcohol is 1 (1.3-1.5) to 15-20.
Further, in the step (1), the concentration of the KOH methanol solution is 2-3mol/L, and the dosage of the KOH methanol solution is 1.2-1.5 times of the mass of the 2, 3-dimercaptosuccinic acid.
Further, in the step (1), the mass ratio of vanillin, the sulfhydryl-containing compound, the absolute ethyl alcohol and DOPO is 1 (2.0-2.5): 5-7): 1.4-1.6.
Further, in the step (2), the mass ratio of the graphene oxide aqueous solution to the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the N-hydroxysuccinimide is 1 (0.012-0.015): (0.010-0.012), and the concentration of the graphene oxide aqueous solution is 10mg/mL.
Further, in the step (2), the mass ratio of the oleylamine to the ethanol to the deionized water is 1 (15-20): 10-20%, and the mass of the oleylamine is 1-3% of the mass of the graphene oxide aqueous solution.
In the step (3), the mass ratio of the graphene oxide containing double bonds, the modified DOPO and the photoinitiator is 1 (2-4) to 0.3-0.5.
Further, the photoinitiator is 2-hydroxy-2-methyl propiophenone.
Further, the process conditions of ultraviolet irradiation are that the irradiation wavelength is 360-400nm, the irradiation time is 0.5-2.0h, and the irradiation intensity is 20-35mW/cm 2.
Further, the preparation method of the modified ammonium polyphosphate comprises the following steps:
uniformly mixing ammonium polyphosphate, dopamine hydrochloride and deionized water, adding Tris-HCl, regulating the pH=8.5 of a system by ammonia water, stirring for 24-36h, centrifuging, washing and drying to obtain modified ammonium polyphosphate.
Further, the mass ratio of the ammonium polyphosphate, the dopamine hydrochloride, the Tris-HCl and the deionized water is 1 (0.1-0.2), 0.05-0.10 and 15-20.
In the technical scheme, under the condition of weak base, the dopamine is oxidized and self-polymerized to form polydopamine, the polydopamine can be deposited on the surface of any material, and the polyphenol structure of polydopamine is not only a good char forming agent, but also has good free radical capturing effect in the combustion process, so that the combustion reaction is inhibited, and the flame retardant property is enhanced.
Further, the compatilizer is at least one of hydrogenated styrene-butadiene-styrene copolymer grafted glycidyl methacrylate, ethylene-methyl acrylate grafted glycidyl methacrylate and styrene-acrylonitrile copolymer grafted glycidyl methacrylate.
Further, the antioxidant is antioxidant 1010.
Further, the extrusion equipment has a first zone temperature of 285-305 ℃, a second zone temperature of 295-315 ℃, a third zone temperature of 295-315 ℃, a fourth zone temperature of 300-320 ℃ and a fifth zone temperature of 290-300 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. According to the flame-retardant high-strength insulating material and the preparation process thereof, 2-chloro-4, 6-diamino-1, 3, 5-triazine and 2, 3-dimercaptosuccinic acid are used for reaction under a strong alkali condition to obtain the mercapto-containing compound, the mercapto-containing compound not only has stability of a triazine structure and excellent carbonization effect, but also is rich in amino and mercapto groups, and is convenient for subsequent chemical reaction, the vanillin, the mercapto-containing compound and DOPO react to obtain modified DOPO, nitrogen, sulfur and phosphorus elements in the modified DOPO can strengthen the flame-retardant property of the modified DOPO to form an effective carbonization layer, flame propagation is slowed down, the thermal stability and the flame-retardant mechanism of the material are positively influenced, long-chain oleylamine is grafted on graphene oxide, the obtained double-bond-containing graphene oxide is improved in hydrophobicity and mechanical property, graphene oxide is not easy to agglomerate, the dispersibility of the graphene oxide is improved, the strength and toughness of the material are further improved, and finally, the rest mercapto groups in the modified DOPO and the double-bond-containing graphene oxide undergo a mercapto-click reaction to form a strong covalent bond, so that the modified DOPO has better overall mechanical property and better flame-retardant property.
2. According to the flame-retardant high-strength insulating material and the preparation process thereof, the core-shell flame retardant integrating flame retardance and reinforcement is prepared by taking ammonium polyphosphate as an acid source, polydopamine as a char forming agent and modified graphene oxide as a reinforcing agent. Through depositing the polydopamine on the surface of the ammonium polyphosphate, then utilizing the acting forces such as hydrogen bond and pi-pi conjugation between the modified graphene oxide and polydopamine, and the like, the modified graphene oxide is assembled on the surface of the polydopamine, so that the effective combination of the ammonium polyphosphate and the modified graphene oxide is realized, the formed core-shell structure can effectively inhibit the propagation of flame, simultaneously, the heat release rate of the material is reduced, the fire resistance grade of the material is increased, and the flame retardant effect is further improved.
3. According to the flame-retardant high-strength insulating material and the preparation process thereof, polyvinyl chloride and crosslinked polyethylene are used as base materials of the insulating material, and an ethylene-vinyl acetate copolymer, a flame retardant, talcum powder, calcium carbonate, a compatilizer and an antioxidant are added to obtain the insulating material. The material has excellent comprehensive properties such as electrical insulation property, flame retardance, heat resistance, impact resistance, tensile strength and the like. The polyvinyl chloride resin is polymerized with the crosslinked polyethylene resin with excellent electric insulation effect and large current-carrying capacity, so that the electric insulation effect and the loading capacity of the composite material can be effectively improved, the flexibility and the mechanical damage resistance of the material are further improved by adding the ethylene-vinyl acetate copolymer, the safety of the material in a high-temperature and flame environment is ensured by using the flame retardant, the cost of the material is reduced by using talcum powder and calcium carbonate as the filler, the rigidity and the heat resistance of the material are enhanced, and the uniformity and the long-term stability of each component are ensured by using the compatilizer and the antioxidant.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment, the graphene oxide is of the type DN-20DY, and is derived from Zhejiang Zhi Nami micro new materials Co., ltd., the ammonium polyphosphate is of the type A823395, and is derived from Shanghai Michelin Biochemical technologies Co., ltd., the polyvinyl chloride is of the type SG-3, the crosslinked polyethylene is of the type SX-0670, the ethylene-vinyl acetate copolymer is of the type P815474, and is derived from Shanghai Michelin Biochemical technologies Co., ltd., the talcum powder is of the particle size of 3000 meshes, the calcium carbonate is of the particle size of 1250 meshes, the compatilizer is ethylene-methyl acrylate grafted glycidyl methacrylate, the E-MA-GMA, the type BF-7L and the antioxidant is of the antioxidant 1010.
In the following examples and comparative examples 1 part equals 10g.
Example 1A preparation process of a flame retardant high strength insulating material comprises the following steps:
step S1, dispersing 5 parts of modified graphene oxide in 450 parts of absolute ethyl alcohol by ultrasonic, adding 15 parts of modified ammonium polyphosphate, uniformly mixing, and performing rotary steaming, washing and drying to obtain a flame retardant;
step S2, uniformly mixing 50 parts of polyvinyl chloride, 20 parts of crosslinked polyethylene, 10 parts of ethylene-vinyl acetate copolymer, 20 parts of flame retardant, 5 parts of talcum powder, 10 parts of calcium carbonate, 6 parts of compatilizer and 3 parts of antioxidant to obtain a mixture, and putting the mixture into extrusion equipment for mixing, extruding and granulating to obtain an insulating material (the temperature of a first area of the extrusion equipment is 285 ℃, the temperature of a second area is 295 ℃, the temperature of a third area is 295 ℃, the temperature of a fourth area is 300 ℃ and the temperature of a fifth area is 290 ℃);
the preparation method of the modified graphene oxide comprises the following steps:
Uniformly mixing 16 parts of 2-chloro-4, 6-diamino-1, 3, 5-triazine and 240 parts of absolute ethyl alcohol, dripping 20.8 parts of 2, 3-dimercaptosuccinic acid and 25 parts of 2mol/L KOH methanol solution, reacting for 20min at 70 ℃ for 24h, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing 10 parts of vanillin, 20 parts of sulfhydryl-containing compound and 50 parts of absolute ethyl alcohol under the protection of nitrogen, reacting for 8h at 65 ℃, adding 14 parts of DOPO, continuously reacting for 10h, and performing rotary steaming, washing and drying to obtain modified DOPO;
Mixing 500 parts of a10 mg/mL graphene oxide aqueous solution, 6 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 5 parts of N-hydroxysuccinimide, performing ultrasonic dispersion for 30min, adding a mixed solution of 5 parts of oleylamine, 225 parts of ethanol and 150 parts of deionized water, continuing ultrasonic dispersion for 2h, stirring for 22h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
Uniformly mixing 5 parts of graphene oxide containing double bonds, 10 parts of modified DOPO and 1.5 parts of photoinitiator, and carrying out ultraviolet irradiation (irradiation wavelength is 360nm, irradiation time is 0.5h, and irradiation intensity is 20mW/cm 2) to obtain modified graphene oxide;
The preparation method of the modified ammonium polyphosphate comprises the following steps:
Uniformly mixing 20 parts of ammonium polyphosphate, 2 parts of dopamine hydrochloride and 300 parts of deionized water, adding 1 part of Tris-HCl, regulating the pH=8.5 of a system by using ammonia water, stirring for 24 hours, and centrifuging, washing and drying to obtain the modified ammonium polyphosphate.
Example 2A preparation process of a flame retardant high strength insulating material comprises the following steps:
step S1, 10 parts of modified graphene oxide is dispersed in 1000 parts of absolute ethyl alcohol by ultrasonic, 20 parts of modified ammonium polyphosphate is added and mixed uniformly, and the flame retardant is obtained after rotary steaming, washing and drying;
Step S2, uniformly mixing 55 parts of polyvinyl chloride, 30 parts of crosslinked polyethylene, 12 parts of ethylene-vinyl acetate copolymer, 30 parts of flame retardant, 10 parts of talcum powder, 15 parts of calcium carbonate, 8 parts of compatilizer and 5 parts of antioxidant to obtain a mixture, and putting the mixture into extrusion equipment for mixing, extruding and granulating to obtain an insulating material (the temperature of one area of the extrusion equipment is 290 ℃, the temperature of the second area is 300 ℃, the temperature of the third area is 305 ℃, the temperature of the fourth area is 310 ℃ and the temperature of the fifth area is 295 ℃);
the preparation method of the modified graphene oxide comprises the following steps:
Uniformly mixing 34 parts of 2-chloro-4, 6-diamino-1, 3, 5-triazine and 620 parts of absolute ethyl alcohol, dripping 48 parts of 2, 3-dimercaptosuccinic acid and 62 parts of 2.5mol/L KOH methanol solution for 30min, reacting at 75 ℃ for 26h, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing 20 parts of vanillin, 48 parts of sulfhydryl-containing compound and 120 parts of absolute ethyl alcohol under the protection of nitrogen, reacting at 70 ℃ for 9h, adding 30 parts of DOPO, continuously reacting for 11h, and performing rotary steaming, washing and drying to obtain modified DOPO;
mixing 1000 parts of a 10mg/mL graphene oxide aqueous solution, 13 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 11 parts of N-hydroxysuccinimide, performing ultrasonic dispersion for 40min, adding a mixed solution of 20 parts of oleylamine, 720 parts of ethanol and 600 parts of deionized water, continuing ultrasonic dispersion for 2.5h, stirring for 23h, centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
uniformly mixing 10 parts of graphene oxide containing double bonds, 30 parts of modified DOPO and 4 parts of photoinitiator, and performing ultraviolet irradiation (irradiation wavelength is 380nm, irradiation time is 1h, and irradiation intensity is 30mW/cm 2) to obtain modified graphene oxide;
The preparation method of the modified ammonium polyphosphate comprises the following steps:
uniformly mixing 20 parts of ammonium polyphosphate, 3 parts of dopamine hydrochloride and 360 parts of deionized water, adding 1.6 parts of Tris-HCl, regulating the pH value of a system to be 8.5 by ammonia water, stirring for 30 hours, and centrifuging, washing and drying to obtain the modified ammonium polyphosphate.
Example 3A preparation process of a flame retardant high strength insulating material comprises the following steps:
step S1, 15 parts of modified graphene oxide is dispersed in 1650 parts of absolute ethyl alcohol by ultrasonic, 25 parts of modified ammonium polyphosphate is added and mixed uniformly, and the flame retardant is obtained after rotary steaming, washing and drying;
Step S2, uniformly mixing 60 parts of polyvinyl chloride, 40 parts of crosslinked polyethylene, 15 parts of ethylene-vinyl acetate copolymer, 40 parts of flame retardant, 15 parts of talcum powder, 20 parts of calcium carbonate, 12 parts of compatilizer and 8 parts of antioxidant to obtain a mixture, and putting the mixture into extrusion equipment for mixing, extruding and granulating to obtain an insulating material (the temperature of one area of the extrusion equipment is 305 ℃, the temperature of the second area is 315 ℃, the temperature of the third area is 315 ℃, the temperature of the fourth area is 320 ℃ and the temperature of the fifth area is 300 ℃);
the preparation method of the modified graphene oxide comprises the following steps:
Uniformly mixing 67 parts of 2-chloro-4, 6-diamino-1, 3, 5-triazine and 1340 parts of absolute ethyl alcohol, dripping 100.5 parts of 2, 3-dimercaptosuccinic acid and 3mol/L KOH methanol solution for 40min, reacting at 80 ℃ for 28h, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing 40 parts of vanillin, 100 parts of sulfhydryl-containing compound and 280 parts of absolute ethyl alcohol under the protection of nitrogen, reacting at 75 ℃ for 10h, adding 64 parts of DOPO, continuously reacting for 12h, and performing rotary steaming, washing and drying to obtain modified DOPO;
Mixing 1500 parts of a 10mg/mL graphene oxide aqueous solution, 22.5 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 18 parts of N-hydroxysuccinimide, performing ultrasonic dispersion for 60min, adding a mixed solution of 45 parts of oleylamine, 900 parts of ethanol and 900 parts of deionized water, continuing ultrasonic dispersion for 3h, stirring for 24h, centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
Uniformly mixing 15 parts of graphene oxide containing double bonds, 60 parts of modified DOPO and 7.5 parts of photoinitiator, and performing ultraviolet irradiation (irradiation wavelength is 360-400nm, irradiation time is 2.0h, and irradiation intensity is 35mW/cm 2) to obtain modified graphene oxide;
The preparation method of the modified ammonium polyphosphate comprises the following steps:
Mixing 25 parts of ammonium polyphosphate, 5 parts of dopamine hydrochloride and 500 parts of deionized water uniformly, adding 2.5 parts of Tris-HCl, regulating the pH value of a system to be 8.5 by ammonia water, stirring for 36 hours, and centrifuging, washing and drying to obtain the modified ammonium polyphosphate.
Comparative example 1 a process for preparing a flame retardant high strength insulating material comprising the following steps:
In comparison to example 2, comparative example 1 replaced modified ammonium polyphosphate with an equivalent mass of ammonium polyphosphate, and the other steps were the same as in example 2.
Comparative example 2A process for preparing a flame retardant high strength insulating material comprising the following steps:
in comparative example 2, the mass ratio of the modified graphene oxide to the modified ammonium polyphosphate was 3:1 as compared with example 2, and the other steps were the same as in example 2.
Comparative example 3a process for preparing a flame retardant high strength insulating material comprising the following steps:
Comparative example 3 the modified graphene oxide was replaced with the same mass of graphene oxide as example 2, except that the procedure was the same as example 2.
Comparative example 4A process for preparing a flame retardant high strength insulating material comprising the following steps:
the preparation method of the modified graphene oxide comprises the following steps:
Uniformly mixing 34 parts of 2-chloro-4, 6-diamino-1, 3, 5-triazine and 620 parts of absolute ethyl alcohol, dripping 48 parts of 2, 3-dimercaptosuccinic acid and 62 parts of 2.5mol/L KOH methanol solution for 30min, reacting at 75 ℃ for 26h, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing 20 parts of vanillin, 48 parts of sulfhydryl-containing compound and 120 parts of absolute ethyl alcohol under the protection of nitrogen, reacting at 70 ℃ for 9h, adding 30 parts of DOPO, continuously reacting for 11h, and performing rotary steaming, washing and drying to obtain modified DOPO;
mixing 1000 parts of a 10mg/mL graphene oxide aqueous solution, 13 parts of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 11 parts of N-hydroxysuccinimide, performing ultrasonic dispersion for 40min, adding a mixed solution of 20 parts of oleylamine, 720 parts of ethanol and 600 parts of deionized water, continuing ultrasonic dispersion for 2.5h, stirring for 23h, centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
Uniformly mixing 10 parts of graphene oxide containing double bonds, 5 parts of modified DOPO and 4 parts of photoinitiator, and performing ultraviolet irradiation (irradiation wavelength is 380nm, irradiation time is 1h, and irradiation intensity is 30mW/cm 2) to obtain modified graphene oxide;
the mass ratio of the double bond-containing graphene oxide to the modified DOPO in comparative example 4 was 1:0.5 as compared with example 2, and the other steps were the same as in example 2.
The insulating materials obtained in examples 1 to 3 and comparative examples 1 to 4 were taken to prepare samples, the properties of which were examined and the examination results were recorded, respectively:
The tensile strength was measured according to GB/T1040.3-2006 test for tensile Properties of plastics, the sample size was 150 mm. Times.15 mm. Times.1 mm, and the tensile speed was 100mm/min.
The oxygen index was determined according to GB/T2406 standard, with a sample size of 125mm by 6.5mm by 3mm.
Test results
| Tensile Strength/MPa | Oxygen index/% | |
| Example 1 | 16.4 | 30 |
| Example 2 | 16.6 | 31 |
| Example 3 | 16.5 | 30 |
| Comparative example 1 | 15.2 | 26 |
| Comparative example 2 | 15.8 | 27 |
| Comparative example 3 | 14.7 | 24 |
| Comparative example 4 | 16.0 | 28 |
From the data in the above table, the following conclusions can be clearly drawn:
1. Compared with examples 1-3, the tensile strength and oxygen index of the product obtained in comparative example 1 are reduced, which shows that the bonding force of the ammonium polyphosphate and the modified graphene oxide can be improved by depositing polydopamine on the surface of the ammonium polyphosphate, so that the mechanical property and the flame retardant property of the material are improved.
2. Compared with examples 1-3, the tensile strength and the oxygen index of the products obtained in comparative examples 2 and 3 are reduced, and the excessive modified graphene oxide occupies the binding site of modified ammonium polyphosphate, so that effective binding is reduced, the performance of the material is affected, and compared with graphene oxide, the modified graphene oxide prepared by the method has better flame retardant effect.
3. Compared with examples 1-3, the tensile strength and the oxygen index of the product obtained in comparative example 4 are both reduced, and it is known that the performance of the modified graphene oxide prepared by the method is influenced by the ratio of each reagent in the preparation process, and the mass ratio in the range is selected, so that the prepared material has excellent flame retardant performance.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation process of a flame-retardant high-strength insulating material is characterized by comprising the following steps:
step S1, ultrasonically dispersing modified graphene oxide in absolute ethyl alcohol, adding modified ammonium polyphosphate, uniformly mixing, and performing rotary steaming, washing and drying to obtain a flame retardant;
and S2, uniformly mixing polyvinyl chloride, crosslinked polyethylene, ethylene-vinyl acetate copolymer, flame retardant, talcum powder, calcium carbonate, compatilizer and antioxidant to obtain a mixture, and putting the mixture into extrusion equipment for mixing, extruding and granulating to obtain the insulating material.
2. The preparation process of the flame-retardant high-strength insulating material according to claim 1, wherein the insulating material comprises, by weight, 50-60 parts of polyvinyl chloride, 20-40 parts of crosslinked polyethylene, 10-15 parts of ethylene-vinyl acetate copolymer, 20-40 parts of flame retardant, 5-15 parts of talcum powder, 10-20 parts of calcium carbonate, 6-12 parts of compatilizer and 3-8 parts of antioxidant.
3. The preparation process of the flame-retardant high-strength insulating material according to claim 2, wherein the flame retardant comprises, by weight, 5-10 parts of modified graphene oxide and 15-30 parts of modified ammonium polyphosphate.
4. The process for preparing the flame-retardant high-strength insulating material according to claim 3, wherein the preparation method of the modified graphene oxide is as follows:
Uniformly mixing 2-chloro-4, 6-diamino-1, 3, 5-triazine and absolute ethyl alcohol, dripping 2, 3-dimercaptosuccinic acid and KOH methanol solution, finishing dripping for 20-40min, reacting for 24-28h at 70-80 ℃, filtering, washing and drying to obtain a sulfhydryl-containing compound, uniformly mixing vanillin, the sulfhydryl-containing compound and absolute ethyl alcohol under the protection of nitrogen, reacting for 8-10h at 65-75 ℃, adding DOPO, continuously reacting for 10-12h, and performing rotary steaming, washing and drying to obtain modified DOPO;
Mixing graphene oxide aqueous solution, 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, performing ultrasonic dispersion for 30-60min, adding a mixed solution of oleylamine, ethanol and deionized water, continuing ultrasonic dispersion for 2-3h, stirring for 22-24h, and centrifuging, filtering and drying to obtain graphene oxide containing double bonds;
and (3) uniformly mixing the graphene oxide containing double bonds, the modified DOPO and the photoinitiator, and irradiating with ultraviolet to obtain the modified graphene oxide.
5. The process for preparing the flame-retardant high-strength insulating material according to claim 4, wherein in the step (3), the mass ratio of the graphene oxide containing double bonds, the modified DOPO and the photoinitiator is 1 (2-4) (0.3-0.5).
6. The process for preparing the flame-retardant high-strength insulating material according to claim 3, wherein the preparation method of the modified ammonium polyphosphate is as follows:
uniformly mixing ammonium polyphosphate, dopamine hydrochloride and deionized water, adding Tris-HCl, regulating the pH=8.5 of a system by ammonia water, stirring for 24-36h, centrifuging, washing and drying to obtain modified ammonium polyphosphate.
7. The process for preparing the flame-retardant high-strength insulating material according to claim 6, wherein the mass ratio of the ammonium polyphosphate to the dopamine hydrochloride to the Tris-HCl to the deionized water is 1 (0.1-0.2) (0.05-0.10) (15-20).
8. The process for preparing a flame retardant high strength insulation material according to claim 2, wherein the compatibilizer is at least one of hydrogenated styrene-butadiene-styrene copolymer grafted glycidyl methacrylate, ethylene-methyl acrylate grafted glycidyl methacrylate, and styrene-acrylonitrile copolymer grafted glycidyl methacrylate.
9. The process for preparing the flame-retardant high-strength insulating material according to claim 2, wherein the antioxidant is antioxidant 1010.
10. A flame retardant, high strength insulating material made according to any one of claims 1-9.
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