WO2022057210A1 - 一种具有ntc效应的聚酰胺组合物及其制备方法 - Google Patents
一种具有ntc效应的聚酰胺组合物及其制备方法 Download PDFInfo
- Publication number
- WO2022057210A1 WO2022057210A1 PCT/CN2021/078174 CN2021078174W WO2022057210A1 WO 2022057210 A1 WO2022057210 A1 WO 2022057210A1 CN 2021078174 W CN2021078174 W CN 2021078174W WO 2022057210 A1 WO2022057210 A1 WO 2022057210A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- iodide
- polyamide composition
- polyamide
- ntc effect
- toluenesulfonamide
- Prior art date
Links
- 239000004952 Polyamide Substances 0.000 title claims abstract description 45
- 229920002647 polyamide Polymers 0.000 title claims abstract description 45
- 239000000203 mixture Substances 0.000 title claims abstract description 38
- 230000000694 effects Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 5
- 239000006229 carbon black Substances 0.000 claims abstract description 19
- 229910001511 metal iodide Inorganic materials 0.000 claims abstract description 16
- 239000004014 plasticizer Substances 0.000 claims abstract description 13
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract 2
- -1 fluorosulfonic acid compound Chemical class 0.000 claims description 23
- 239000003963 antioxidant agent Substances 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- IPRJXAGUEGOFGG-UHFFFAOYSA-N N-butylbenzenesulfonamide Chemical group CCCCNS(=O)(=O)C1=CC=CC=C1 IPRJXAGUEGOFGG-UHFFFAOYSA-N 0.000 claims description 10
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- LMYRWZFENFIFIT-UHFFFAOYSA-N toluene-4-sulfonamide Chemical compound CC1=CC=C(S(N)(=O)=O)C=C1 LMYRWZFENFIFIT-UHFFFAOYSA-N 0.000 claims description 8
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical group I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 claims description 8
- YYROPELSRYBVMQ-UHFFFAOYSA-N 4-toluenesulfonyl chloride Chemical compound CC1=CC=C(S(Cl)(=O)=O)C=C1 YYROPELSRYBVMQ-UHFFFAOYSA-N 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 5
- WNSXUAGCWVZDQC-UHFFFAOYSA-N n-ethylbenzenesulfonamide Chemical compound CCNS(=O)(=O)C1=CC=CC=C1 WNSXUAGCWVZDQC-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- KHBQMWCZKVMBLN-UHFFFAOYSA-N Benzenesulfonamide Chemical compound NS(=O)(=O)C1=CC=CC=C1 KHBQMWCZKVMBLN-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 3
- DKYVVNLWACXMDW-UHFFFAOYSA-N n-cyclohexyl-4-methylbenzenesulfonamide Chemical compound C1=CC(C)=CC=C1S(=O)(=O)NC1CCCCC1 DKYVVNLWACXMDW-UHFFFAOYSA-N 0.000 claims description 3
- OHPZPBNDOVQJMH-UHFFFAOYSA-N n-ethyl-4-methylbenzenesulfonamide Chemical compound CCNS(=O)(=O)C1=CC=C(C)C=C1 OHPZPBNDOVQJMH-UHFFFAOYSA-N 0.000 claims description 3
- QKIWHADSHFVRFN-UHFFFAOYSA-N n-propan-2-ylbenzenesulfonamide Chemical compound CC(C)NS(=O)(=O)C1=CC=CC=C1 QKIWHADSHFVRFN-UHFFFAOYSA-N 0.000 claims description 3
- WFRUBUQWJYMMRQ-UHFFFAOYSA-M potassium;1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [K+].[O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F WFRUBUQWJYMMRQ-UHFFFAOYSA-M 0.000 claims description 3
- YFSUTJLHUFNCNZ-UHFFFAOYSA-M 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-M 0.000 claims description 2
- YCMLQMDWSXFTIF-UHFFFAOYSA-N 2-methylbenzenesulfonimidic acid Chemical compound CC1=CC=CC=C1S(N)(=O)=O YCMLQMDWSXFTIF-UHFFFAOYSA-N 0.000 claims description 2
- 239000004953 Aliphatic polyamide Substances 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 claims description 2
- 229920003231 aliphatic polyamide Polymers 0.000 claims description 2
- KWQLUUQBTAXYCB-UHFFFAOYSA-K antimony(3+);triiodide Chemical compound I[Sb](I)I KWQLUUQBTAXYCB-UHFFFAOYSA-K 0.000 claims description 2
- 229940075417 cadmium iodide Drugs 0.000 claims description 2
- AVWLPUQJODERGA-UHFFFAOYSA-L cobalt(2+);diiodide Chemical compound [Co+2].[I-].[I-] AVWLPUQJODERGA-UHFFFAOYSA-L 0.000 claims description 2
- GBRBMTNGQBKBQE-UHFFFAOYSA-L copper;diiodide Chemical compound I[Cu]I GBRBMTNGQBKBQE-UHFFFAOYSA-L 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 150000004677 hydrates Chemical class 0.000 claims description 2
- BQZGVMWPHXIKEQ-UHFFFAOYSA-L iron(ii) iodide Chemical compound [Fe+2].[I-].[I-] BQZGVMWPHXIKEQ-UHFFFAOYSA-L 0.000 claims description 2
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 claims description 2
- AOJBACHWNDMRQP-UHFFFAOYSA-N n,n-diethyl-4-methylbenzenesulfonamide Chemical compound CCN(CC)S(=O)(=O)C1=CC=C(C)C=C1 AOJBACHWNDMRQP-UHFFFAOYSA-N 0.000 claims description 2
- SIIWTWXTZDDNTI-UHFFFAOYSA-N n-(2-hydroxyethyl)-4-methylbenzenesulfonamide Chemical compound CC1=CC=C(S(=O)(=O)NCCO)C=C1 SIIWTWXTZDDNTI-UHFFFAOYSA-N 0.000 claims description 2
- QHUJTQAJBPYVQF-UHFFFAOYSA-N n-(2-hydroxyethyl)benzenesulfonamide Chemical compound OCCNS(=O)(=O)C1=CC=CC=C1 QHUJTQAJBPYVQF-UHFFFAOYSA-N 0.000 claims description 2
- DHRXPBUFQGUINE-UHFFFAOYSA-N n-(2-hydroxypropyl)benzenesulfonamide Chemical compound CC(O)CNS(=O)(=O)C1=CC=CC=C1 DHRXPBUFQGUINE-UHFFFAOYSA-N 0.000 claims description 2
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 claims description 2
- 229920006012 semi-aromatic polyamide Polymers 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 claims description 2
- QPBYLOWPSRZOFX-UHFFFAOYSA-J tin(iv) iodide Chemical compound I[Sn](I)(I)I QPBYLOWPSRZOFX-UHFFFAOYSA-J 0.000 claims description 2
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 15
- 229920000642 polymer Polymers 0.000 abstract description 6
- 238000005485 electric heating Methods 0.000 abstract description 4
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003078 antioxidant effect Effects 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 229920001778 nylon Polymers 0.000 description 10
- 239000004677 Nylon Substances 0.000 description 9
- 229920000571 Nylon 11 Polymers 0.000 description 3
- 229920006659 PA12 Polymers 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
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- 229910021389 graphene Inorganic materials 0.000 description 2
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- 238000000034 method Methods 0.000 description 2
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- VBCUEUULCJFHAZ-VKHMYHEASA-N (4S)-4-amino-5-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctylsulfonyloxy)-5-oxopentanoic acid Chemical compound OC(=O)CC[C@H](N)C(=O)OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F VBCUEUULCJFHAZ-VKHMYHEASA-N 0.000 description 1
- QSRJVOOOWGXUDY-UHFFFAOYSA-N 2-[2-[2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]ethoxy]ethoxy]ethyl 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCCOCCOCCOC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 QSRJVOOOWGXUDY-UHFFFAOYSA-N 0.000 description 1
- SSADPHQCUURWSW-UHFFFAOYSA-N 3,9-bis(2,6-ditert-butyl-4-methylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C)=CC(C(C)(C)C)=C1OP1OCC2(COP(OC=3C(=CC(C)=CC=3C(C)(C)C)C(C)(C)C)OC2)CO1 SSADPHQCUURWSW-UHFFFAOYSA-N 0.000 description 1
- NSNHWGDFYDLMBS-UHFFFAOYSA-N 4-(3-hydroxypropyl)benzenesulfonamide Chemical compound NS(=O)(=O)C1=CC=C(CCCO)C=C1 NSNHWGDFYDLMBS-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
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- 101000576320 Homo sapiens Max-binding protein MNT Proteins 0.000 description 1
- 102000004310 Ion Channels Human genes 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
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- 150000001413 amino acids Chemical class 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
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- 229920006119 nylon 10T Polymers 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229920006128 poly(nonamethylene terephthalamide) Polymers 0.000 description 1
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- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 description 1
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- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
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- 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
- C08K3/16—Halogen-containing compounds
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/43—Compounds containing sulfur bound to nitrogen
- C08K5/435—Sulfonamides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
- G01K7/22—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a non-linear resistance, e.g. thermistor
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
一种具有NTC效应的聚酰胺组合物及其制备方法,所述具有NTC效应的聚酰胺组合物其重量份包括以下组份:聚酰胺树脂100份;金属碘化物0.05-3份;氟磺酸化合物0.1-5份;增塑剂0-15份;炭黑0.1-1.5份;其它助剂0-1份。制备得到的具有NTC效应的聚酰胺组合物是一种良好的聚合物基热敏电阻材料(NTC材料),且在低温条件下断裂伸长率高,通电稳定性变高,组合物的热稳定性高,可以用于电热毯、电热坐垫、暖风垫、电热板取暖器、电壁炉和车座加热器等电取暖器等领域中。
Description
本发明属于高分子聚合物领域,特别涉及一种具有NTC效应的聚酰胺组合物及其制备方法。
NTC(Negative Temperature Coefficient)是负(零下)温度系数。NTC材料是指随温度上升电阻呈指数关系减小、具有负温度系数的热敏电阻现象和材料。1834年,科学家首次发现了硫化银有负温度系数的特性。1930年,科学家发现氧化亚铜-氧化铜也具有负温度系数的性能,并将之成功地运用在航空仪器的温度补偿电路中。随后,由于晶体管技术的不断发展,热敏电阻器的研究取得重大进展。
近年来,有文献指出聚合物基负温度系数温敏电阻材料(Negative Temperature coefficient,简称NTC),它是以聚合物材料为基体,加入炭黑、金属粉、金属氧化物等导电填料,经过分散复合等后处理后而形成的多相复合体系,其电阻率具有随温度升高而降低的特点,NTC温敏电阻主要用于测量和电子电路的温度补偿。
现有技术中,以对苯乙烯磺酸钠接枝的石墨烯或负载纳米银的石墨烯为导电填料制备了聚偏氟乙烯基温敏电阻材料,但是存在导电相填充高、室温电阻率偏大、灵敏度偏低等问题。
现有技术中,为了提升尼龙制品的NTC效应,一般会在尼龙中填充较高含量的碘化锌等含碘化合物,该体系虽然具有较好的热敏传导性,但高比例的金属碘化物和金属氧化物的使用会降低尼龙材料的韧性和可加工性和力学性能。
本领域中,长期存在着聚合物基热敏电阻材料(NTC)存在成型性能较差,加工困难等问题。
发明内容
本发明的目的通过全氟磺酸盐促进金属碘化物的分散形成较好的离子通道,从而形成一种具有NTC效应的聚酰胺组合物,也就是一种良好的聚合物基热敏电阻材料(NTC材料),在低温条件下断裂生长率高,且通电稳定性高,组合物的热稳定性高。
进一步地,本发明还提供上述具有NTC效应的聚酰胺组合物的制备方法。
一种具有NTC效应的聚酰胺组合物,包括以下组份:
优选地,具有NTC效应的聚酰胺组合物,按其重量份包括以下组份:
优选地,具有NTC效应的聚酰胺组合物,按其重量份包括以下组份:
更优选地,具有NTC效应的聚酰胺组合物,按其重量份包括以下组份:
优选地,所述的聚酰胺树脂选自脂肪族聚酰胺、半芳香族聚酰胺、聚内酰胺中的至少一种。
优选地,所述金属碘化物和氟磺酸化合物的重量比是0.4-10,更优选地,所述金属碘化物和氟磺酸化合物的重量比是2-7.5,更优选的,所述金属碘化物和氟磺酸化合物的重量比是2.5-7.5。
所述聚酰胺可以选自通过缩聚至少一种脂肪族二元羧酸与至少一种脂肪族二胺或者环二胺获得的聚酰胺,例如PA6,PA66,PA610、PA612、PA56,PA46,MXD6、PA510、PA11、PA12、PA1010、PA1012、PA1212;或者通过缩聚至少一种芳香族二羧酸与至少一种脂肪族二胺获得的聚酰胺,例如聚对苯二甲酰胺、聚间苯二甲酰胺、聚芳酰胺,具体是PA9T、PA10T;或者通过至少一种氨基酸或内酰胺与其本身的缩聚所获得的聚酰胺,例如PA6,PA7,PA11,PA12;或者它们的混合物或共聚酰胺。
更优选地,所述聚酰胺树脂优选熔点在150℃-230℃的尼龙材料,如PA11,PA12,PA1012,PA1212。所述的尼龙材料,在100ml的溶液中的0.5g尼龙,测量的相对粘度在2.0-2.5之间。
优选地,所述金属碘化物选自碘化锌,碘化锡,碘化锑,碘化铜,碘化镍,碘化锰,碘化钴,碘化铁,碘化铅,碘化镉,碘化钛,碘化钠,碘化钾以及它们的水合物中的至少一种化合物。
优选地,所述氟磺酸化合物选自全氟辛烷磺酸胺、全氟辛烷磺酸钾、全氟辛烷磺酸四乙胺和全氟辛烷磺酰氨谷氨酸钾中的一种或多种。
其中,所述炭黑的BET比表面积为2-200m
2/g,优选炭黑的BET比表面积为65-110m
2/g,比表面积的测试法为GB/T 19587-2017《气体吸附BET法测定固态物质比表面积》,炭黑吸油值(DBP)吸收为50-300ml/100g,选择DBP>120ml/100g的炭黑有利于静电耗散,按照标准GB/T3780.2-2017进行炭黑吸油值的检测。
其中,所述的增塑剂选自N-丁基苯磺酰胺(BBSA)、对甲苯磺酰胺(PTSA)、邻对甲苯磺酰胺(O/PTSA)、对甲苯磺酰氯(PTSC)、N-(2-羟丙基)苯磺酰胺(HPBSA)、N-乙基邻对甲苯磺酰胺(N-E-O/PTSA)、N-乙基对甲苯磺酰胺(N-E-PTSA)、甲苯磺酰胺甲醛树脂(MH/MS)、甲苯磺酰胺甲醛树脂醋酸丁酯溶液(MS-80)、N-环已基对甲苯磺酰胺(CTSA)、N,N-二乙基对甲苯磺酰胺(DETSA)、N-乙基苯磺酰胺(EBSA)、N-异丙基苯磺酰胺(IBSA)、N-烷基对甲苯磺酰胺(TTSA)、N-(2-羟乙基)苯磺酰胺、N,N-双(2-羟乙基)对甲苯磺酰胺、N-(2-羟乙基)对甲苯磺酰胺、苯磺酰胺(BSA)其中的一个或者多个。
所述其它助剂包括抗氧剂、润滑剂中的至少一种。
所述抗氧剂选自受阻酚和亚磷酸酯类抗氧剂,比如抗氧剂1010,抗氧剂1098,抗氧剂1079,抗氧剂245和抗氧剂168,抗氧剂MD-1024,抗氧剂PEP-36,抗氧剂P-EPQ,抗氧剂626,抗氧剂627AV等。
所述润滑剂选自润滑剂EBS或润滑剂硬脂酸锌。
进一步地,一种制备如上所述的具有NTC效应的聚酰胺组合物的制备方法,按比例将聚酰胺树脂、金属碘化物、氟磺酸化合物、增塑剂、炭黑和其它助剂混合均匀,并通过双螺杆挤出机挤出造粒,制得具有NTC效应的聚酰胺组合物。
相较于现有技术,本发明制得的具有NTC效应的聚酰胺组合物具备温度响应特征,,本发明在聚酰胺树脂中添加金属磺化物、氟磺酸化合物、炭黑和增塑剂,特定金属碘化物和特定氟磺酸化合物在特定比例下,和炭黑与增塑剂的共同作用下,可以使得在添加低比例的金属碘化物,制得具有NTC效应的聚酰胺组合物,是一种良好的聚合物基热敏电阻材料(NTC材料),可以广泛应用于电热毯、电热坐垫、暖风垫、电热板取暖器、电壁炉和车座加热器等电取暖器等领域中。
图1为性能测试的电阻线示意图。
为了使本技术领域的人员更好地理解本发明方案,下面结合具体实施例对本发明作进一步的详细说明。
PA1212:无锡殷达尼龙有限公司,熔点是183℃;
PA66:50BWFS,ASCED科技有限公司,熔点265℃;
碘化锌,碘化钾:分析纯,上海阿拉丁生化科技股份有限公司;
炭黑1:ENSACO,E250G,比表面积为65m
2/g,DBP值为190ml/100g,益瑞石中国有限公司;
炭黑2:ENSACO,E350G,比表面积为770m
2/g,DBP值为220ml/100g,益瑞石中国有限公司;
炭黑3:HIBLACK 50L,比表面积为110m
2/g,DBP值为40ml/100g:Deguss化工;
增塑剂:N-丁基苯磺酰胺(BBSA),N-乙基苯磺酰胺(EBSA),菏泽市嘉联生物科技有限 公司;
全氟辛烷磺酸钾PFBS-A:FC-98,武汉赛沃尔化工有限公司;
抗氧剂:利安隆,RIANOX MD-1024;
其余原料均来自市售。
实施例1-14
按表1所示的重量份备料,将聚酰胺、金属碘化物、氟磺酸化合物、增塑剂、炭黑和抗氧剂混合均匀,并通过螺杆公称直径为40mm双螺杆挤出机挤出造粒,制得聚酰胺组合物。
对比例1
按表1所示的重量份备料,将聚酰胺、金属碘化物、增塑剂、炭黑和抗氧剂混合均匀,并通过螺杆公称直径为40mm双螺杆挤出机挤出造粒,制得聚酰胺组合物。
对比例2
按表1所示的重量份备料,将聚酰胺、氟磺酸化合物、增塑剂、炭黑和抗氧剂混合均匀,并通过螺杆公称直径为40mm双螺杆挤出机挤出造粒,制得聚酰胺组合物。
对比例3-5
按表1所示的重量份备料,将聚酰胺、金属碘化物、氟磺酸化合物、增塑剂、炭黑和抗氧剂混合均匀,并通过螺杆公称直径为40mm双螺杆挤出机挤出造粒,制得聚酰胺组合物。
对比例6
按表1所示的重量份备料,将聚酰胺、金属碘化物、氟磺酸化合物、增塑剂和抗氧剂混合均匀,并通过螺杆公称直径为40mm双螺杆挤出机挤出造粒,制得聚酰胺组合物。
性能测试
将实施例和对比例制得的聚酰胺组合物,通过挤出制得厚度为0.8mm的线缆,采用如附图1所示的电阻线示意图,1是聚酯芯线(直径1.2mm,采用相对粘度为1.0的PET为基础的芯线),2是铜合金电极线(厚度0.3mm,铜镍含量为98:2),3是尼龙热敏层(0.8mm),4是铜合金电极线(厚度0.3mm,铜镍含量为98:2),5.耐热PVC外层(0.8mm,耐热等级为105℃的PVC电缆线,常州安内特电缆有限公司提供)。挤出的多层线缆,在-30℃下对折,然后将线外层剥开,观察对折处的尼龙层的状态。
参考GB/T666.3-2007(直热式负温度系数热敏电阻器)这个国家标准采用哈克单螺杆挤出机挤出直径为1mm厚的片材,截取70mm×70mm×1mm的片材,在片材两端连接上高阻仪,高阻仪的型号为PROSTAT@PRC-801,配以恒温烘箱,测试在不同温度下 70mm×70mm×1mm的片材电阻的变化。在上述片材两端加10V-100的电压,将上述片材两端至于烘箱中30min,设定烘箱温度分别为30℃和70℃,测试绝缘材料电阻的变化,列于表2中。
按照标准ISO 525 1BA注塑成0.75mm的拉伸样品,按照50mm/min的速度拉伸,测得拉伸强度和断裂伸长率,分别列于表2和表3中。
表1实施例和对比例配方表
表2聚酰胺组合物的性能测试表-1
表3聚酰胺组合物的性能测试表-2
对比例1 | 对比例2 | 对比例3 | 对比例4 | 对比例5 | 对比例6 | |
电阻1/欧(30℃) | 93000 | 46000 | 9420 | 8730 | 6700 | 93000 |
电阻2/欧(70℃) | 37000 | 10300 | 4930 | 3210 | 2300 | 7800 |
断裂伸长率(%) | 73 | 68 | 40 | 35 | 90 | 70 |
-30℃下180°弯折,观察尼龙层的变化 | 不开裂 | 不开裂 | 开裂 | 开裂 | 不开裂 | 不开裂 |
NTC效应(电阻1/电阻2) | 2.5 | 4.4 | 1.9 | 2.7 | 2.9 | 12 |
实验结果表明,高含量的无机物的添加会影响材料低温下的断裂伸长率,本发明制得的具有NTC效应的聚酰胺组合物,NTC效应值落在20-60之间;其断裂伸长率高,特别是在低温环境下弯折不容易产生开裂现象。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (11)
- 如权利要求2所述的具有NTC效应的聚酰胺组合物,其特征在于:所述金属碘化物和氟磺酸化合物的重量比是0.4-10。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述的聚酰胺树脂选自脂肪族聚酰胺、半芳香族聚酰胺、聚内酰胺中的至少一种。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述聚酰胺树脂选自熔点为150℃-230℃的聚酰胺。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述金属碘化物选自碘化锌、碘化锡、碘化锑、碘化铜、碘化镍、碘化锰、碘化钴、碘化铁、碘化铅、碘化镉、碘化钛、碘化钠和碘化钾及其水合物中的至 少一种化合物。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述氟磺酸化合物选自全氟辛烷磺酸胺、全氟辛烷磺酸钾、全氟辛烷磺酸四乙胺和全氟辛烷磺酰氨谷氨酸钾中的一种或多种。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述炭黑的BET比表面积为2-200m 2/g,标准的DBP吸收为50-300ml/100g。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述的增塑剂选自N-丁基苯磺酰胺、对甲苯磺酰胺、邻对甲苯磺酰胺、对甲苯磺酰氯、N-(2-羟丙基)苯磺酰胺、N-乙基邻对甲苯磺酰胺、N-乙基对甲苯磺酰胺、甲苯磺酰胺甲醛树脂、甲苯磺酰胺甲醛树脂醋酸丁酯溶液、N-环已基对甲苯磺酰胺、N,N-二乙基对甲苯磺酰胺、N-乙基苯磺酰胺、N-异丙基苯磺酰胺、N-烷基对甲苯磺酰胺、N-(2-羟乙基)苯磺酰胺、N,N-双(2-羟乙基)对甲苯磺酰胺,N-(2-羟乙基)对甲苯磺酰胺、苯磺酰胺其中的一个或者多个。
- 如权利要求1-3任一项所述的具有NTC效应的聚酰胺组合物,其特征在于:所述其它助剂包括抗氧剂和润滑剂中的至少一种。
- 一种如权利要求1-10任一所述的具有NTC效应的聚酰胺组合物的制备方法:按比例将聚酰胺树脂、金属碘化物、氟磺酸化合物、增塑剂、炭黑和其它助剂混合均匀,并通过双螺杆挤出机挤出造粒,制得具有NTC效应的聚酰胺组合物。
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US9175146B2 (en) * | 2006-08-08 | 2015-11-03 | Sabic Global Technologies B.V. | Thermal conductive polymeric PTC compositions |
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US20140205336A1 (en) * | 2013-01-18 | 2014-07-24 | Samsung Electronics Co., Ltd. | Resistance heating element and heating member and fusing device employing the same |
CN104497394A (zh) * | 2014-12-11 | 2015-04-08 | 郑州大学 | 具有负温度系数效应的聚合物基温敏电阻材料及其制备方法 |
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