CN112876809A - Outer insulating protective material of cable - Google Patents
Outer insulating protective material of cable Download PDFInfo
- Publication number
- CN112876809A CN112876809A CN202110053428.2A CN202110053428A CN112876809A CN 112876809 A CN112876809 A CN 112876809A CN 202110053428 A CN202110053428 A CN 202110053428A CN 112876809 A CN112876809 A CN 112876809A
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- China
- Prior art keywords
- product
- ketone
- reaction
- sulfone
- heating
- Prior art date
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- Granted
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000001681 protective effect Effects 0.000 title claims abstract description 20
- 229920001643 poly(ether ketone) Polymers 0.000 claims abstract description 56
- 150000003457 sulfones Chemical class 0.000 claims abstract description 38
- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 37
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 37
- 238000009413 insulation Methods 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 20
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims abstract description 8
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003086 colorant Substances 0.000 claims abstract description 8
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 69
- 239000000047 product Substances 0.000 claims description 63
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 29
- 239000002250 absorbent Substances 0.000 claims description 28
- 230000002745 absorbent Effects 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 22
- 238000010992 reflux Methods 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 238000002390 rotary evaporation Methods 0.000 claims description 12
- ZXDDPOHVAMWLBH-UHFFFAOYSA-N 2,4-Dihydroxybenzophenone Chemical compound OC1=CC(O)=CC=C1C(=O)C1=CC=CC=C1 ZXDDPOHVAMWLBH-UHFFFAOYSA-N 0.000 claims description 11
- IUNJCFABHJZSKB-UHFFFAOYSA-N 2,4-dihydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C(O)=C1 IUNJCFABHJZSKB-UHFFFAOYSA-N 0.000 claims description 10
- ROLLGPMWNMQJCX-UHFFFAOYSA-N 4-(2-nitroethenyl)benzene-1,3-diol Chemical compound OC1=CC=C(C=C[N+]([O-])=O)C(O)=C1 ROLLGPMWNMQJCX-UHFFFAOYSA-N 0.000 claims description 10
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- PLVUIVUKKJTSDM-UHFFFAOYSA-N 1-fluoro-4-(4-fluorophenyl)sulfonylbenzene Chemical compound C1=CC(F)=CC=C1S(=O)(=O)C1=CC=C(F)C=C1 PLVUIVUKKJTSDM-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 8
- 239000012065 filter cake Substances 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 6
- UESSEMPSSAXQJC-UHFFFAOYSA-N ethanol;methanamine Chemical compound NC.CCO UESSEMPSSAXQJC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 6
- 229920002866 paraformaldehyde Polymers 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- ZDYVRSLAEXCVBX-UHFFFAOYSA-N pyridinium p-toluenesulfonate Chemical compound C1=CC=[NH+]C=C1.CC1=CC=C(S([O-])(=O)=O)C=C1 ZDYVRSLAEXCVBX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- CZKLEJHVLCMVQR-UHFFFAOYSA-N 4-fluorobenzoyl chloride Chemical compound FC1=CC=C(C(Cl)=O)C=C1 CZKLEJHVLCMVQR-UHFFFAOYSA-N 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 230000004224 protection Effects 0.000 claims description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 5
- -1 sulfuryl phenyl Chemical group 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 claims description 4
- WPFVBOQKRVRMJB-UHFFFAOYSA-N hydroxycitronellal Chemical compound O=CCC(C)CCCC(C)(C)O WPFVBOQKRVRMJB-UHFFFAOYSA-N 0.000 claims description 4
- IOXXVNYDGIXMIP-UHFFFAOYSA-N n-methylprop-2-en-1-amine Chemical compound CNCC=C IOXXVNYDGIXMIP-UHFFFAOYSA-N 0.000 claims description 4
- KFSKETMKJUKOTJ-UHFFFAOYSA-N phenyl-(6-sulfonylcyclohexa-2,4-dien-1-yl)methanone Chemical class C=1C=CC=CC=1C(=O)C1C=CC=CC1=S(=O)=O KFSKETMKJUKOTJ-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000004440 column chromatography Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- NQMRYBIKMRVZLB-UHFFFAOYSA-N methylamine hydrochloride Chemical compound [Cl-].[NH3+]C NQMRYBIKMRVZLB-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005292 vacuum distillation Methods 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N monoethanolamine hydrochloride Natural products NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 28
- 125000001174 sulfone group Chemical group 0.000 abstract description 17
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 7
- 229920000587 hyperbranched polymer Polymers 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 31
- 238000010521 absorption reaction Methods 0.000 description 21
- 238000004458 analytical method Methods 0.000 description 9
- 125000003277 amino group Chemical group 0.000 description 8
- 125000003172 aldehyde group Chemical group 0.000 description 7
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 4
- 150000001336 alkenes Chemical group 0.000 description 4
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 230000006750 UV protection Effects 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000012801 ultraviolet ray absorbent Substances 0.000 description 3
- 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 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- KZTYYGOKRVBIMI-UHFFFAOYSA-N diphenyl sulfone Chemical group C=1C=CC=CC=1S(=O)(=O)C1=CC=CC=C1 KZTYYGOKRVBIMI-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 150000002576 ketones Chemical group 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 1
- RAAGZOYMEQDCTD-UHFFFAOYSA-N 2-fluorobenzoyl chloride Chemical compound FC1=CC=CC=C1C(Cl)=O RAAGZOYMEQDCTD-UHFFFAOYSA-N 0.000 description 1
- LSQARZALBDFYQZ-UHFFFAOYSA-N 4,4'-difluorobenzophenone Chemical group C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 LSQARZALBDFYQZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WLLGXSLBOPFWQV-UHFFFAOYSA-N MGK 264 Chemical compound C1=CC2CC1C1C2C(=O)N(CC(CC)CCCC)C1=O WLLGXSLBOPFWQV-UHFFFAOYSA-N 0.000 description 1
- 150000001263 acyl chlorides Chemical group 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000005902 aminomethylation reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000008365 aromatic ketones Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000006332 fluoro benzoyl group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 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
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 125000006239 protecting group Chemical group 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols
- C08G65/40—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives derived from phenols from phenols (I) and other compounds (II), e.g. OH-Ar-OH + X-Ar-X, where X is halogen atom, i.e. leaving group
- C08G65/4012—Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones
- C08G65/4056—(I) or (II) containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polyethers (AREA)
Abstract
The invention discloses a cable outer layer insulation protective material which comprises the following components in parts by weight: 72-77 parts of polyether-ether-ketone, 16-18 parts of aminated sulfone-based hybrid polyether ketone, 4-5 parts of modified ultraviolet absorber, 2-4 parts of dioctyl phthalate and 0.7-1.3 parts of colorant. The hyperbranched polymer is prepared by mixing polyether-ether-ketone and aminated sulfone-based hybrid polyether-ketone, wherein a large number of branched chain structures are introduced to aminated sulfone-based hybrid polyether-ketone chains through amino addition, so that the flexibility of the polymer is improved, the prepared product has higher toughness, the impact strength is improved, and meanwhile sulfone groups are introduced into the molecular chains of the hyperbranched polymer, so that the molecular chain regularity is reduced due to the large volume of the sulfone groups, and the impact strength of the molecules is further improved.
Description
Technical Field
The invention belongs to the field of cable preparation, and relates to an outer-layer insulation protective material for a cable.
Background
The PEEK has the characteristics of good coating processability, good flame retardance, stable insulation, hydrolysis resistance, compression resistance, corrosion resistance and easiness in coloring, is widely applied to preparation of cable insulation protective materials, but has poor impact strength, and can be modified by filling, blending, crosslinking, grafting and other methods to obtain a PEEK plastic alloy or a PEEK composite material with more excellent performance in order to further improve the performance of the PEEK so as to meet comprehensive performance and diversified requirements in various fields. Patent No. CN103275458B discloses a polyether ether ketone cable material and a method for manufacturing the same, which is prepared by blending polyether ether ketone, polyester ether, polyphenylene oxide and carboximide, but when the polyether ether ketone is directly mixed with polyether ester, the mechanical properties of the material after the polyether ester is added will be reduced because the dispersibility of the two is reduced by mechanical mixing.
Disclosure of Invention
The invention aims to provide a cable outer layer insulation protection material which is prepared by mixing polyether-ether-ketone and aminated sulfone-based hybrid polyether-ketone, wherein a large number of branched structures are introduced to an aminated sulfone-based hybrid polyether-ketone chain through amino addition, so that the flexibility of a polymer is improved, the prepared product has higher toughness, the impact strength is improved, a modified ultraviolet absorbent is introduced through a grafting reaction, long-chain alkyl and silane groups are introduced to the modified ultraviolet absorbent, the toughness of the polymer is improved, the aminated sulfone-based hybrid polyether-ketone hyperbranched structure is similar to the polyether-ether-ketone structure, so that the compatibility between the aminated sulfone-based hybrid polyether-ketone and the polyether-ether-ketone is enhanced, the adhesive force between the aminated sulfone-based hybrid polyether-ketone and the polyether-ether-ketone is improved, and the strength of the polymer is further improved due to the introduction of a large number of triazine ring groups in the aminated sulfone-based hybrid polyether-, and the tensile strength of the polymer is not reduced while the toughness of the polymer is enhanced, and meanwhile, sulfone groups are introduced into the molecular chain of the hyperbranched polymer, so that the molecular chain regularity is reduced due to the large volume of the sulfone groups, and the impact strength of the molecules is further improved.
The purpose of the invention can be realized by the following technical scheme:
the cable outer layer insulation protective material comprises the following components in parts by weight:
72-77 parts of polyether-ether-ketone, 16-18 parts of aminated sulfone-based hybrid polyether ketone, 4-5 parts of modified ultraviolet absorber, 2-4 parts of dioctyl phthalate and 0.7-1.3 parts of colorant;
the specific preparation process of the aminated sulfuryl hybrid polyether ketone comprises the following steps:
step 1: firstly, mixing and dissolving ethanol and methylamine hydrochloride according to the mass ratio of 1.5:1, then adding sodium carbonate into the mixture, stirring the mixture, standing the mixture, filtering the mixture, washing filter residues with ethanol to ensure that the pH value of the washing solution and the filtrate is 9 after the washing solution and the filtrate are combined to obtain a methylamine ethanol solution, then adding 2, 4-dihydroxybenzaldehyde and ethanol into a reaction tank, stirring the mixture for dissolving, adding nitromethane and the prepared methylamine ethanol solution, stirring the mixture for 3 to 4 hours at room temperature, heating the mixture to reflux, reacting for 6 to 7 hours, filtering the mixture, washing a filter cake with ethanol, and drying the filter cake to obtain 4- (2-nitrovinyl) benzene-1, 3-diol;
preferably, 3.5 to 3.6mL of ethanol and 1.28 to 1.31g of nitromethane are added into each gram of 2, 4-dihydroxy benzaldehyde;
step 2: simultaneously adding 4,4' -difluorodiphenyl sulfone, p-fluorobenzoyl chloride and a mixed solvent into a reaction kettle, stirring and heating to 60 ℃, adding aluminum chloride into the reaction kettle in several times, heating to 120 ℃, keeping the temperature and reacting for 4-5 hours, quickly pouring a product into a mixture of concentrated hydrochloric acid and ice water, stirring, filtering and washing with water, then pouring the product into a saturated sodium bicarbonate solution, heating to a condensation rate, and washing with water to be neutral to obtain the polyfluorinated sulfuryl benzophenone; acyl chloride groups in fluorobenzoyl chloride can perform acylation reaction with ortho-positions of fluorine elements in 4,4 '-difluorodiphenyl sulfone, so that ortho-positions of two phenyl groups of 4,4' -difluorodiphenyl sulfone are introduced into fluorobenzoyl, and due to the steric hindrance influence, the two introduction directions are opposite, so that four fluorine atoms in a prepared intermediate product B are in four different directions, the prepared intermediate product B takes a phenylsulfone group as a center, two phenylketone groups are introduced into two sides, and the introduction of the phenylsulfone group improves the flexibility and the impact resistance of a polymer;
preferably, 1.34-1.37g of p-fluorobenzoyl chloride is added into each gram of 4,4' -difluorodiphenyl sulfone, 10-11mL of mixed solvent is added, and 1.95-1.97g of aluminum chloride is added; the mixed solvent is prepared by mixing dimethyl sulfoxide and sulfolane according to the mass ratio of 1: 1;
and step 3: continuously introducing nitrogen into the reaction kettle for 10min, adding 4- (2-nitrovinyl) benzene-1, 3-diol, polyfluorinated sulfuryl phenyl ketone, potassium carbonate, toluene and N-methyl pyrrolidone into the reaction kettle, heating to reflux for reaction for 2-3h, removing the toluene, heating to 200-210 ℃ for reaction for 6-7h, pouring the product into a mixed solution of water and hydrochloric acid according to a ratio of 12:1, stirring and filtering, washing a filter cake with deionized water, and drying to obtain branched sulfuryl hybrid polyether ketone;
preferably, 1.09-1.1kg of 4- (2-nitrovinyl) benzene-1, 3-diol, 198-201g of potassium carbonate, 410-415g of sodium carbonate are added per kg of the polyfluorinated sulfuryl benzophenone;
and 4, step 4: adding branched sulfonyl hybrid polyether ketone into dimethyl sulfoxide, stirring and dissolving, then adding melamine and pyridine, heating to 70-80 ℃, reacting for 8-10h, keeping the temperature unchanged, adding ammonia water into the mixture, reacting for 2-3h, performing rotary evaporation on the product to remove the solvent, and washing and drying the product with hot water to obtain aminated sulfonyl hybrid polyether ketone; the branched sulfonyl hybrid polyether ketone is a hyperbranched structure, because 4- (2-nitrovinyl) benzene-1, 3-diol is positioned at a terminal group, a large number of olefin group action sites are uniformly distributed at the terminal, the interior of a molecular chain also contains olefin groups, and simultaneously the olefin groups are connected with nitro groups which strongly attract electrons, so that the branched sulfonyl hybrid polyether ketone has high activity and can react with amino groups in melamine, so that the hyperbranched sulfonyl hybrid polyether ketone terminal group is introduced into melamine groups, and amino groups are introduced, so that the olefin groups which are difficult to react due to steric hindrance can react with amine in ammonia, so that a large number of amino groups are uniformly introduced into a prepared product, and simultaneously, due to the internal branched structure of the branched sulfonyl hybrid polyether ketone, the regularity of a polymer is reduced, the melting point is reduced, and the processing performance is improved, the hyperbranched structure of the polymer enhances the compatibility between the polymer and the polyether-ether-ketone, reduces the chain winding of polyether-ether-ketone molecules, further improves the processing resistance of the composite product, enhances the compatibility with other additives, and simultaneously introduces sulfone groups into the molecular chain of the hyperbranched polymer, reduces the molecular chain regularity due to large size of the sulfone groups, and further improves the molecular toughness;
preferably, 7-8L of dimethyl sulfoxide is added into each kilogram of branched sulfone group hybridized polyether ketone, 120g of melamine 115-ketone is added, and 600mL of pyridine is added;
the preparation process of the modified ultraviolet absorbent is as follows:
s1: adding hydroxycitronellal, ethylene glycol, pyridinium p-toluenesulfonate and toluene into a reaction kettle at the same time, refluxing and dividing water until no water is generated, carrying out rotary evaporation to recover the toluene, adding a sodium bicarbonate solution with the mass concentration of 5% into a product, stirring and mixing, extracting with ethyl acetate, combining organic phases, drying with anhydrous sodium sulfate, removing the solvent under reduced pressure, and then separating by column chromatography to obtain a product A;
preferably, 1.16-1.19mol of ethylene glycol, 0.05mol of pyridinium p-toluenesulfonate and 750mL of toluene 700-;
s2, simultaneously adding the product A, dimethylchlorosilane and petroleum ether into a reaction kettle, heating to 90-100 ℃, performing reflux reaction for 3-4h, evaporating to remove the petroleum ether, and performing vacuum distillation to obtain a product B;
preferably, the product A and the dimethylchlorosilane are added according to the mass ratio of 1: 1.09-1.1;
s3: adding the product B and N-allylmethylamine into a reaction kettle at the same time, adding a chloroplatinic acid isopropanol solution with the concentration of 0.1mol/L into the reaction kettle, heating to 80-85 ℃ for refluxing, monitoring the reaction process by using a gas chromatograph in the reaction process, and performing reduced pressure distillation after the reaction is completed to obtain a product C;
preferably, 1.1-1.2mol of N-allylmethylamine is added into each mol of the product B, and 0.55-0.58mL of 0.1mol/L isopropanol chloroplatinic acid solution is added;
s4: adding 2, 4-dihydroxybenzophenone, paraformaldehyde and ethanol into a reaction kettle, stirring and dissolving, then adding a product C into the reaction kettle, heating to 50-60 ℃ for reaction for 2h, heating to 80-90 ℃ for reflux reaction for 6-7h, performing rotary evaporation to remove a solvent and unreacted substances, washing the product with water at 40 ℃, and drying to obtain a product D, wherein hydrogen on a para-carbon atom of a phenolic hydroxyl group in the 2, 4-dihydroxybenzophenone has certain activity and can perform aminomethylation reaction with an amino compound under the action of paraformaldehyde, so that the product C is introduced into the 2, 4-dihydroxybenzophenone;
preferably, 1.1 to 1.2mol of the product C is added into each mol of 2, 4-dihydroxybenzophenone, and 30 to 32g of paraformaldehyde is added;
s5: simultaneously adding the product D, acetone, water and p-toluenesulfonic acid into a reaction kettle, heating to 65-70 ℃, carrying out reflux reaction for 4-5h, quenching the reaction by using a saturated sodium bicarbonate solution, carrying out rotary evaporation on the product, washing with water, and drying to obtain a modified ultraviolet absorbent, and introducing two aldehyde groups into the product after removing protective groups;
preferably, 22-25mL of acetone, 3mL of water and 43-46mg of p-toluenesulfonic acid are added to each gram of the product D;
a preparation process of a cable outer layer insulation protective material comprises the following specific preparation processes: and adding the aminated sulfone-based hybrid polyether ketone and the modified ultraviolet absorbent into a 270-280 ℃ internal mixer at the same time, mixing for 15-20min, discharging, adding the obtained material, polyether ether ketone, dioctyl phthalate and a colorant into a double-screw extruder at the same time, and extruding and granulating to obtain the cable outer layer insulation protective material. Although the aminated sulfuryl hybrid polyether ketone is added through amino, a certain amount of double bonds still exist, because the double bonds are easy to oxidize, and the bond of C-S bond on sulfuryl in the molecule is lower than C-C bond, and the double bonds are easy to decompose under the action of ultraviolet ray and further cause oxidation, the aminated sulfuryl hybrid polyether ketone contains amino, and can react with aldehyde group in the modified ultraviolet ray absorbent during melting and mixing to generate C ═ N bond, so that the modified ultraviolet ray absorbent is uniformly coated on the surface of the three-dimensional ellipsoid structure, because the modified ultraviolet ray absorbent contains 2, 4-dihydroxybenzophenone group, the aminated sulfuryl hybrid polyether ketone has high ultraviolet ray absorption performance, can absorb ultraviolet ray and prevent the oxidation of the polymer, and simultaneously the generated C ═ N bond and the triazine ring form a conjugated structure to cause the enhancement of the rigidity of the polymer, the flexibility decreases but the flexibility of the polymer increases by introducing a long-chain flexible group siloxane bond on the modified uv absorber chain.
The invention has the beneficial effects that:
1. the material is prepared by mixing polyether-ether-ketone and aminated sulfone-based hybrid polyether-ketone, wherein a large number of branched structures are introduced to aminated sulfone-based hybrid polyether-ketone chains through amino addition, so that the flexibility of the polymer is improved, the prepared product has higher toughness and improved impact strength, and a modified ultraviolet absorbent is introduced through a grafting reaction, wherein long-chain alkyl and silane groups are introduced to the modified ultraviolet absorbent, so that the toughness of the polymer is improved, and the compatibility between the aminated sulfone-based hybrid polyether-ketone hyperbranched structure and the polyether-ether-ketone structure is enhanced due to the similarity of the aminated sulfone-based hybrid polyether-ketone hyperbranched structure and the polyether-ether-ketone structure, so that the adhesion between the aminated sulfone-based hybrid polyether-ketone and the polyether-ether-ketone is improved, and meanwhile, the strength of the polymer is further improved due to the introduction of a large number of triazine ring groups in, and the tensile strength of the polymer is not reduced while the toughness of the polymer is enhanced, and meanwhile, sulfone groups are introduced into the molecular chain of the hyperbranched polymer, so that the molecular chain regularity is reduced due to the large volume of the sulfone groups, and the impact strength of the molecules is further improved.
2. The prepared aminated sulfone-based hybrid polyether ketone contains amino, and can react with aldehyde groups in the modified ultraviolet absorbent during melting and mixing, so that the modified ultraviolet absorbent can be uniformly coated on the surface of a three-dimensional ellipsoid structure, the modified ultraviolet absorbent has high ultraviolet absorption performance due to the 2, 4-dihydroxybenzophenone groups, and can absorb ultraviolet rays and prevent the oxidation of a polymer, and the modified ultraviolet absorbent is directly grafted on the polymer through reaction, so that the modified ultraviolet absorbent is uniformly dispersed, and the prepared aminated sulfone-based hybrid polyether ketone has high ultraviolet resistance and is not easy to be oxidized.
Detailed Description
Please refer to the following examples for details:
(1) examples and comparative examples of preparation of aminated branched polyether ether ketones
Example 1:
the specific preparation process of the aminated branched polyether-ether-ketone comprises the following steps:
step 1: firstly, 0.5g of ethanol and 0.33g of methylamine hydrochloride are mixed and dissolved, then 0.5g of sodium carbonate is added into the mixture, the mixture is stirred and statically filtered, filter residues are washed by the ethanol, the pH value of the combined washing solution and the filtrate is 9, a methylamine ethanol solution is obtained, then 10g of 2, 4-dihydroxy benzaldehyde and 36mL of ethanol are added into a reaction tank, the mixture is stirred and dissolved, then 13g of nitromethane and the methylamine ethanol solution are added, the mixture is stirred for 3 to 4 hours at room temperature, the mixture is heated to reflux, then the mixture reacts for 6 to 7 hours, filtered, filter cakes are washed by the ethanol and dried, and 4- (2-nitrovinyl) benzene-1, 3-diol is obtained, and infrared analysis shows that 1532cm-1Occurrence of-NO2Absorption peak 1607cm-1C ═ C absorption peak occurs;
step 2: simultaneously adding 10g of 4,4' -difluorodiphenyl sulfone, 13.5g of p-fluorobenzoyl chloride, 50mL of dimethyl sulfoxide and 50mL of sulfolane into a reaction kettle, stirring and heating to 60 ℃, adding 19.6g of aluminum chloride into the reaction kettle in three times, wherein the adding amount is the same for each time, adding the time interval of 20min, then heating to 120 ℃, carrying out heat preservation reaction for 5h, quickly pouring the product into a mixture of concentrated hydrochloric acid and ice water, stirring, filtering and washing with water, then pouring the product into a saturated sodium bicarbonate solution, heating and reducing the rate of washing with water to be neutral, and obtaining the polyfluorinated sulfonyl benzophenone; by infrared analysis, 1142 and 1593cm-1Is the absorption peak of sulfone group S ═ O, 1650cm-1Is the absorption peak of the arone group;
and step 3: continuously introducing nitrogen into the reaction kettle for 10min, adding 11g of 4- (2-nitrovinyl) benzene-1, 3-diol, 10g of polyfluorinated sulfuryl phenyl ketone, 2g of potassium carbonate, 4.1g of sodium carbonate, 32mL of toluene and 75 mLN-methyl pyrrolidone into the reaction kettle, heating to reflux for reaction for 3h, removing the toluene, heating to 210 ℃ for reaction for 7h, pouring the product into a mixed solution of water and hydrochloric acid according to a ratio of 12:1, stirring and filtering, and using deionized water to filter a filter cakeWashing and drying to obtain aminated sulfone-based hybrid polyether ketone; the infrared analysis shows that 1161cm-1In the form of-O-absorption peaks at 1146 and 1591cm-1The absorption peak is the sulfonyl S ═ O, 1605cm-1Has a C-C absorption peak at 1652cm-1Has aromatic ketone absorption peak of 3197cm-1Has an-OH absorption peak;
and 4, step 4: adding 10g of aminated sulfone-based hybrid polyether ketone into 75mL of dimethyl sulfoxide, stirring and dissolving, then adding 1.2g of melamine and 60mL of pyridine, heating to 70 ℃ for reaction for 10h, then keeping the temperature unchanged, adding 4.6g of ammonia water into the mixture for reaction for 3h, performing rotary evaporation on the product to remove the solvent in the product, washing with hot water and drying to obtain aminated sulfone-based hybrid polyether ketone, wherein infrared analysis shows that the concentration of the aminated sulfone-based hybrid polyether ketone is 3362cm-1And 3211cm-1With primary amine C-NH2Absorption peak of 816, 1438, 1551cm-1The infrared absorption peak of the triazine ring appears.
Comparative example 1:
the specific procedure for preparing the sulfone-based hybrid polyetherketone was the same as in example 1, except that the 4- (2-nitrovinyl) benzene-1, 3-diol added in step 2 was replaced with hydroquinone.
Comparative example 2:
the specific procedure for the preparation of the aminated branched polyether ether ketone was the same as in example 1, except that 4,4 '-difluorodiphenyl sulfone added in step 3 was replaced with 4,4' -difluorobenzophenone.
(2) Examples and comparative examples of modified UV absorbers preparation:
example 2:
the preparation process of the modified ultraviolet absorbent is as follows:
s1: adding 1.72g of hydroxycitronellal, 0.73g of ethylene glycol, 0.126g of pyridinium p-toluenesulfonate and 7.5mL of toluene into a reaction kettle at the same time, refluxing for water diversion till no water is generated, carrying out rotary evaporation to recover the toluene, adding a 5% sodium bicarbonate solution into the product, stirring and mixing, extracting with ethyl acetate, combining organic phases, drying with anhydrous sodium sulfate, removing the solvent under reduced pressure, separating by column chromatography to obtain a product A, wherein the infrared analysis shows that the concentration is 1722cm-1The infrared absorption peak of the aldehyde group disappears,reacting ethylene glycol with aldehyde group in pyridinium p-toluenesulfonate;
s2 adding 2.08g of the product A, 1.02g of dimethylchlorosilane and 10mL of petroleum ether into a reaction kettle at the same time, heating to 95 ℃, carrying out reflux reaction for 4 hours, evaporating to remove the petroleum ether, and then carrying out vacuum distillation to obtain a product B, wherein infrared analysis shows that 872cm of the product B-1An infrared absorption peak of Si-O-C appears;
s3: adding 2.65g of the product B and 0.71g of N-allylmethylamine into a reaction kettle at the same time, adding 5.7 mu L of chloroplatinic acid isopropanol solution with the concentration of 0.1mol/L, heating to 85 ℃ for refluxing, monitoring the reaction process by using a gas chromatograph in the reaction process, carrying out reduced pressure distillation after the reaction is completed to obtain a product C, wherein the infrared analysis shows that 1173cm of the product C is-1An absorption peak of C-N is formed;
s4: adding 2.14g of 2, 4-dihydroxybenzophenone, 0.3g of paraformaldehyde and 10mL of ethanol into a reaction kettle, stirring for dissolving, then adding 3.7g of product C into the reaction kettle, heating to 60 ℃, reacting for 2h, heating to 85 ℃, refluxing for reacting for 7h, removing the solvent and unreacted substances by rotary evaporation, washing the product with water at 40 ℃, drying to obtain product D, wherein the infrared analysis shows that the concentration is 3183cm-1Has an infrared absorption peak of 874cm at phenolic hydroxyl-1An infrared absorption peak of Si-O-C appears;
s5: adding 2g of the product D, 45mL of acetone, 6mL of water and 90mg of p-toluenesulfonic acid into a reaction kettle at the same time, heating to 70 ℃, carrying out reflux reaction for 5 hours, quenching the reaction by using a saturated sodium bicarbonate solution, carrying out rotary evaporation on the product, washing by using water, and drying to obtain a modified ultraviolet absorbent, wherein infrared analysis shows that 1724cm-1Infrared absorption peak with aldehyde group at the same time of 3184cm-1Has infrared absorption peak of phenolic hydroxyl.
(3) Examples and comparative examples of the preparation method of the cable outer layer insulation protective material:
example 3:
a preparation process of a cable outer layer insulation protective material comprises the following specific preparation processes: 170g of aminated sulfone-based hybrid polyether ketone and 45g of modified ultraviolet absorbent are simultaneously added into an internal mixer at 270 ℃ for mixing for 15-20min, then discharging is carried out, and the obtained material, 750g of polyether ether ketone, 30g of dioctyl phthalate and 10g of colorant are simultaneously added into a double-screw extruder for extrusion and granulation, so as to obtain the cable outer layer insulation protective material.
Comparative example 3:
a preparation process of a cable outer layer insulation protection material is the same as that in example 3, and the sulfone-based hybrid polyether ketone prepared in example 1 and used in example 3 is replaced by the sulfone-based hybrid polyether ketone prepared in comparative example 1.
Comparative example 4:
a preparation process of a cable outer layer insulation protection material is the same as that in example 3, and the aminated sulfone-based hybrid polyether ketone prepared in example 1 and used in example 3 is replaced with aminated branched polyether ether ketone prepared in comparative example 2.
Comparative example 5:
a preparation process of a cable outer layer insulation protective material is the same as that in example 3, and the modified ultraviolet absorbent used in example 2 and used in example 3 is replaced by 19g2, 4-dihydroxybenzophenone.
Comparative example 6:
a preparation process of a cable outer layer insulation protective material comprises the step of directly adding 750g of polyether-ether-ketone, 170g of polyester ether, 45g of modified ultraviolet absorbent, 30g of dioctyl phthalate and 10g of colorant into a double-screw extruder at the same time for extrusion granulation to obtain the cable outer layer insulation protective material.
Comparative example 7:
a preparation process of a cable outer layer insulation protective material comprises the step of directly adding 750g of polyether-ether-ketone, 45g of a modified ultraviolet absorbent, 30g of dioctyl phthalate and 10g of a coloring agent into a double-screw extruder at the same time for extrusion granulation to obtain the cable outer layer insulation protective material.
Test example:
(1) the materials prepared in example 3, comparative example 4 and comparative example 5 were placed in a xenon weather-resistant test chamber, and the irradiation intensity in the test chamber was controlled to 550W/m2The temperature is 100 ℃, the humidity is 50%, after aging for 80 days, the tensile strength of the material before and after aging is measured according to GB/T1040-2006, and then the attenuation rate of the tensile strength is calculated as (initial tensile strength-tensile strength after aging)/x 100% of the initial tensile strength; the calculation result shows that the tensile strength attenuation rate in example 3 is 3.1%, because the added aminated sulfone-based hybrid polyether ketone contains amino groups, the amino groups can react with aldehyde groups in the modified ultraviolet absorbent during melting and mixing, so that the modified ultraviolet absorbent can uniformly coat the surface of the three-dimensional ellipsoid structure, because the modified ultraviolet absorbent contains 2, 4-dihydroxybenzophenone groups, the modified ultraviolet absorbent has high ultraviolet absorption performance, can absorb ultraviolet rays and prevent oxidation of polymers, and the modified ultraviolet absorbent is directly grafted on the polymers through reaction, so that the modified ultraviolet absorbent is uniformly dispersed, so that the prepared aminated sulfone-based hybrid polyether ketone has high ultraviolet resistance and is not easily oxidized, while the tensile strength attenuation rate in comparative example 3 is 14.6%, because no amino groups are introduced into the added sulfone-based hybrid polyether ketone, further, the added modified ultraviolet absorbent can only be physically stirred and mixed, so that the dispersion is uneven, and the oxidation resistance of the product is reduced; the tensile strength attenuation rate in the comparative example 4 is 2.3%, and the oxidation resistance of the polymer is improved due to the fact that the modified ultraviolet absorbent is directly grafted on the molecular chain to achieve higher ultraviolet resistance, and meanwhile, no sulfone group is introduced on the molecular chain; in the comparative example 5, the tensile strength attenuation rate is 14.2%, 2, 4-dihydroxybenzophenone is directly added into the aminated sulfuryl hybrid polyether ketone, the two cannot react, and the mixture is directly physically stirred and mixed to cause uneven dispersion, so that the product is resistant to the stressThe ultraviolet performance is reduced.
(2) The flame retardant performance of the materials prepared in example 3, comparative example 4 and comparative example 5 was measured, and the flame retardant rating was V-O rating and no dripping phenomenon was observed.
(3) The impact strength of the material of comparative example 7 was determined to be I according to GB/T1843-20080The impact strength of the materials of example 3, comparative example 4, comparative example 5 and comparative example 6 is I1Then, the rate of change of the impact strength of the material (I) was calculated1-I0)/I0X 100%, and the tensile strength of the material of comparative example 7 was determined to be N according to GB/T1040-20060The tensile strength of the materials in example 3, comparative example 4, comparative example 5 and comparative example 6 was N1Then, the rate of change of the tensile strength of the material (N) was calculated1-N0)/N0X 100%, calculated as shown in table 1:
TABLE 1 determination of the impact strength and tensile Strength Change ratio of the materials
As can be seen from table 1, in example 3, the cable material is prepared by compounding the aminated sulfone-based hybrid polyetherketone and the polyetheretherketone, wherein a large number of branched structures are introduced to the aminated sulfone-based hybrid polyetherketone chain through amino addition, so that the flexibility of the polymer is improved, the prepared product has high toughness and improved impact strength, and the modified ultraviolet absorber is introduced through a grafting reaction, wherein a long-chain alkyl group and a silane group are introduced to the modified ultraviolet absorber, so that the toughness of the polymer is improved, and the compatibility between the aminated sulfone-based hybrid polyetherketone and the polyetheretherketone is enhanced due to the hyperbranched structure of the aminated sulfone-based hybrid polyetherketone and the structural similarity with the polyetheretherketone, so that the adhesion between the aminated sulfone-based hybrid polyetherketone and the polyetheretherketone is improved, and the strength of the polymer is further improved due to the introduction of a large number of triazine ring groups in the aminated sulfone-, the tensile strength of the polymer is not reduced while the toughness of the polymer is enhanced, and meanwhile, sulfone groups are introduced into the molecular chain of the hyperbranched polymer, so that the molecular chain regularity is reduced due to the large volume of the sulfone groups, and the toughness of the molecule is further improved; in comparative example 3, branched amino groups are not introduced to the aminated sulfone group hybrid polyether ketone chain, and long-chain modified ultraviolet absorbers are not introduced, so that the toughness is reduced, the impact strength is reduced, meanwhile, triazine ring groups are not introduced, so that the tensile strength is reduced, in comparative example 4, only branched amino groups are introduced, and sulfone groups are not introduced, so that the toughness of the material is reduced, in comparative example 5, long-chain modified ultraviolet absorbers are not introduced to the aminated sulfone group hybrid polyether ketone chain, so that the toughness is reduced, the impact strength is reduced, in comparative example 6, polyether ester is directly added to polyether ether ketone, the toughness of the mixed polyether ether ketone is increased, but the mechanical strength is greatly reduced, and as the compatibility between polyether ether ketone and polyether ester is low, the adhesion between molecules is reduced, the mechanical property is reduced, and the compatibility is low, so that the toughness is not greatly improved after mixing.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. The cable outer layer insulation protective material is characterized by comprising the following components in parts by weight:
72-77 parts of polyether-ether-ketone, 16-18 parts of aminated sulfone-based hybrid polyether ketone, 4-5 parts of modified ultraviolet absorber, 2-4 parts of dioctyl phthalate and 0.7-1.3 parts of colorant;
the specific preparation process of the aminated sulfuryl hybrid polyether ketone comprises the following steps:
step 1: firstly, mixing and dissolving ethanol and methylamine hydrochloride according to the mass ratio of 1.5:1, then adding sodium carbonate into the mixture, stirring the mixture, standing the mixture, filtering the mixture, washing filter residues with ethanol to ensure that the pH value of the washing solution and the filtrate is 9 after the washing solution and the filtrate are combined to obtain a methylamine ethanol solution, then adding 2, 4-dihydroxybenzaldehyde and ethanol into a reaction tank, stirring the mixture for dissolving, adding nitromethane and the prepared methylamine ethanol solution, stirring the mixture for 3 to 4 hours at room temperature, heating the mixture to reflux, reacting for 6 to 7 hours, filtering the mixture, washing a filter cake with ethanol, and drying the filter cake to obtain 4- (2-nitrovinyl) benzene-1, 3-diol;
step 2: simultaneously adding 4,4' -difluorodiphenyl sulfone, p-fluorobenzoyl chloride and a mixed solvent into a reaction kettle, stirring and heating to 60 ℃, adding aluminum chloride into the reaction kettle in batches, heating to 120 ℃, keeping the temperature and reacting for 4-5 hours, quickly pouring a product into a mixture of concentrated hydrochloric acid and ice water, stirring, filtering and washing with water, then pouring the product into a saturated sodium bicarbonate solution, adding hot water and washing to be neutral to obtain the polyfluorinated sulfuryl phenyl ketone;
and step 3: continuously introducing nitrogen into the reaction kettle for 10min, adding 4- (2-nitrovinyl) benzene-1, 3-diol, polyfluorinated sulfuryl phenyl ketone, potassium carbonate, toluene and N-methyl pyrrolidone into the reaction kettle, heating to reflux for reaction for 2-3h, removing the toluene, heating to 200-210 ℃ for reaction for 6-7h, pouring the product into a mixed solution of water and hydrochloric acid according to a ratio of 12:1, stirring and filtering, washing a filter cake with deionized water, and drying to obtain branched sulfuryl hybrid polyether ketone;
and 4, step 4: adding the branched sulfonyl hybrid polyether ketone into dimethyl sulfoxide, stirring and dissolving, then adding melamine and pyridine, heating to 70-80 ℃, reacting for 8-10h, keeping the temperature unchanged, adding ammonia water into the mixture, reacting for 2-3h, performing rotary evaporation on the product to remove the solvent, and washing and drying with hot water to obtain the aminated sulfonyl hybrid polyether ketone.
2. The cable sheath insulating and protecting material according to claim 1, wherein 3.5-3.6mL of ethanol and 1.28-1.31g of nitromethane are added per gram of 2, 4-dihydroxybenzaldehyde in step 1.
3. The cable outer layer insulation protective material according to claim 1, characterized in that in step 2, 1.34-1.37g of p-fluorobenzoyl chloride is added to each gram of 4,4' -difluorodiphenyl sulfone, 10-11mL of mixed solvent is added, and 1.95-1.97g of aluminum chloride is added; the mixed solvent is prepared by mixing dimethyl sulfoxide and sulfolane according to the mass ratio of 1:1.
4. The cable sheath insulating and protecting material as claimed in claim 1, wherein in step 3, 4- (2-nitrovinyl) benzene-1, 3-diol, 198-201g potassium carbonate and 410-415g sodium carbonate are added per kg of the polyfluorinated sulfuryl benzophenone in an amount of 1.09-1.1 kg.
5. The cable outer layer insulation protection material as claimed in claim 1, wherein in step 4, 7-8L of dimethyl sulfoxide, 120g of melamine 115-acetone and 600mL of pyridine are added to each kilogram of branched sulfone-based hybrid polyether ketone.
6. The cable sheath insulation protective material of claim 1, wherein the modified ultraviolet absorber is prepared by the following steps:
s1: adding hydroxycitronellal, ethylene glycol, pyridinium p-toluenesulfonate and toluene into a reaction kettle at the same time, refluxing and dividing water until no water is generated, carrying out rotary evaporation to recover the toluene, adding a sodium bicarbonate solution with the mass concentration of 5% into a product, stirring and mixing, extracting with ethyl acetate, combining organic phases, drying with anhydrous sodium sulfate, removing the solvent under reduced pressure, and then separating by column chromatography to obtain a product A;
s2, simultaneously adding the product A, dimethylchlorosilane and petroleum ether into a reaction kettle, heating to 90-100 ℃, performing reflux reaction for 3-4h, evaporating to remove the petroleum ether, and performing vacuum distillation to obtain a product B;
s3: adding the product B and N-allylmethylamine into a reaction kettle at the same time, adding a chloroplatinic acid isopropanol solution with the concentration of 0.1mol/L into the reaction kettle, heating to 80-85 ℃ for refluxing, monitoring the reaction process by using a gas chromatograph in the reaction process, and performing reduced pressure distillation after the reaction is completed to obtain a product C;
s4: adding 2, 4-dihydroxybenzophenone, paraformaldehyde and ethanol into a reaction kettle, stirring and dissolving, then adding the product C, heating to 50-60 ℃, reacting for 2h, heating to 80-90 ℃, performing reflux reaction for 6-7h, performing rotary evaporation to remove a solvent and unreacted substances, washing the product with water at 40 ℃, and drying to obtain a product D;
s5: and simultaneously adding the product D, acetone, water and p-toluenesulfonic acid into a reaction kettle, heating to 65-70 ℃, carrying out reflux reaction for 4-5h, quenching the reaction by using a saturated sodium bicarbonate solution, carrying out rotary evaporation on the product, washing by using water, and drying to obtain the modified ultraviolet absorbent.
7. The cable sheath insulating and protecting material as claimed in claim 6, wherein in step S1, 1.16-1.19mol of ethylene glycol, 0.05mol of pyridinium p-toluenesulfonate and 750mL of toluene 700-750mL are added to each mol of hydroxycitronellal.
8. The cable sheath insulating and protecting material of claim 6, wherein in step S4, 1.1-1.2mol of the product C is added to each mol of 2, 4-dihydroxybenzophenone, and 30-32g of paraformaldehyde is added.
9. A preparation process of the cable outer layer insulation protection material as claimed in claim 1, which is characterized by comprising the following specific preparation processes: and adding the aminated sulfone-based hybrid polyether ketone and the modified ultraviolet absorbent into a 270-280 ℃ internal mixer at the same time, mixing for 15-20min, discharging, adding the obtained material, polyether ether ketone, dioctyl phthalate and a colorant into a double-screw extruder at the same time, and extruding and granulating to obtain the cable outer layer insulation protective material.
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