CN114940800B - 一种抗静电高阻燃pvc光缆料及其制备方法 - Google Patents
一种抗静电高阻燃pvc光缆料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 230000003287 optical effect Effects 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920000915 polyvinyl chloride Polymers 0.000 title description 55
- 239000004800 polyvinyl chloride Substances 0.000 title description 55
- 229920000734 polysilsesquioxane polymer Polymers 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000005303 weighing Methods 0.000 claims abstract description 17
- -1 acrylic ester Chemical class 0.000 claims abstract description 15
- 239000002608 ionic liquid Substances 0.000 claims abstract description 15
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical group ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920000642 polymer Polymers 0.000 claims abstract description 13
- 239000012265 solid product Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 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 claims abstract description 9
- 239000003063 flame retardant Substances 0.000 claims abstract description 9
- 239000011256 inorganic filler Substances 0.000 claims abstract description 9
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 9
- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 8
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 150000001450 anions Chemical class 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 229920000768 polyamine Polymers 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical group [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 9
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 235000009518 sodium iodide Nutrition 0.000 claims description 4
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 claims description 4
- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 3
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims description 3
- XAMCLRBWHRRBCN-UHFFFAOYSA-N 5-prop-2-enoyloxypentyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCOC(=O)C=C XAMCLRBWHRRBCN-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000001506 calcium phosphate Substances 0.000 claims description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 3
- 235000011010 calcium phosphates Nutrition 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 3
- 235000011009 potassium phosphates Nutrition 0.000 claims description 3
- 229940114930 potassium stearate Drugs 0.000 claims description 3
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- 229920005557 bromobutyl Chemical group 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 125000006038 hexenyl group Chemical group 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 229940096992 potassium oleate Drugs 0.000 claims description 2
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims description 2
- 229940083575 sodium dodecyl sulfate Drugs 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000003245 coal Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 2
- AXFVIWBTKYFOCY-UHFFFAOYSA-N 1-n,1-n,3-n,3-n-tetramethylbutane-1,3-diamine Chemical compound CN(C)C(C)CCN(C)C AXFVIWBTKYFOCY-UHFFFAOYSA-N 0.000 description 1
- GLISZRPOUBOZDL-UHFFFAOYSA-N 3-bromopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCBr GLISZRPOUBOZDL-UHFFFAOYSA-N 0.000 description 1
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 239000012212 insulator Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000013308 plastic optical fiber Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
- C08L51/085—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds on to polysiloxanes
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
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Abstract
本发明公开了一种抗静电高阻燃PVC光缆料的制备方法,其包括以下步骤:S1称取原料共聚单体、去离子水、乳化剂和交联剂;共聚单体为氯乙烯、丙烯酸酯和单乙烯基笼型聚倍半硅氧烷,反应结束后,得到改性PVC预聚体;S2将其与多元胺在催化剂作用下反应,得到固体产物;将其与含阴离子盐搅拌反应,得到含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;S3将其与硅烷偶联剂、纳米无机填料、加工助剂和润滑剂预混后,挤塑后得到抗静电高阻燃PVC光缆料。本发明制备得到的PVC光缆料,不仅具有优异的防静电和阻燃性能,而且具有优异的抗冲击性能和耐低温脆性性能,从而使其满足石化、煤矿等严苛恶劣环境下的使用要求。
Description
技术领域
本发明涉及PVC复合材料的技术领域,尤其涉及一种抗静电高阻燃PVC光缆料及其制备方法。
背景技术
随着我国工业化的高速发展,大量通信光缆得到了广泛的应用,不仅接入小区、商场等低风险场所,而且还接入化工、加油站、煤炭矿井等高危场所。塑料光缆是由单芯或多芯塑料光纤外包覆聚乙烯、聚氯乙烯等塑料护套的传输光信号的导光介质。
但是PVC塑料光缆料是良好的绝缘体,表面电阻大,在使用过程中易集聚电荷,对石化、煤矿井下作业等危险场所带来潜在的安全隐患,例如静电荷积累到一定的程度,就会引起静电吸尘、放电、击穿,从而导致火灾、爆炸等生产安全事故发生。因此,塑料PVC光缆护套通常需要进行改性处理,以提高其抗静电和阻燃性能,从而满足严苛恶劣环境下安全使用的严格要求。
现有技术中,为了提高PVC光缆料的防静电性能,需要在PVC配方中添加大量的导电炭黑。大量导电炭黑的添加,不仅难以在PVC光缆料中均匀分散,而且降低了材料的抗冲击强度,且低温脆性特别明显,难以满足严苛恶劣环境下的PVC材料使用要求。
发明内容
鉴于以上现有技术的不足之处,本发明的目的在于提供一种抗静电高阻燃PVC光缆料及其制备方法,以解决现有PVC光缆料防静电阻燃性能差、抗冲击强度低和低温脆性明显等问题。
为达到以上目的,本发明采用的技术方案为:
一种抗静电高阻燃PVC光缆料的制备方法,所述制备方法包括以下步骤:
S1:按质量比为1:2~3:0.03~0.05:0.01~0.05称取原料共聚单体、去离子水、乳化剂和交联剂,所述共聚单体为氯乙烯和单乙烯基笼型聚倍半硅氧烷,加入适量的引发剂,加热至30~50℃进行反应,反应结束后,真空抽滤,干燥,得到改性PVC预聚体;所述氯乙烯和单乙烯基笼型聚倍半硅氧烷的摩尔比为10~30:1~5;
S2:按重量份计,称取20~50份改性PVC预聚体溶于100份甲苯中,加入7.6~16.8份多元胺和0.1~0.5份催化剂,在60~80℃下搅拌反应1~2h,反应结束,抽滤得到固体产物;称取40~60份固体产物溶于100份乙腈中,再加入3~12份含阴离子盐,在20~30℃搅拌反应15~24h,反应结束后,将所得反应液倒入乙醇中析出沉淀物,所得混合液抽滤、滤饼真空干燥后制得含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;
S3:按重量份计,称取50~100份含离子液体笼型聚倍半硅氧烷改性的PVC聚合物、0.5~2.5份硅烷偶联剂、2~8份纳米无机填料、10~15份加工助剂和5~12份润滑剂预混后,通过165~185℃温度挤塑后得到抗静电高阻燃PVC光缆料。
进一步地,所述单乙烯基笼型聚倍半硅氧烷如化学式I所示
式中,R1为溴丙基或溴丁基,R2为乙烯基、烯丙基或己烯基。
笼型聚倍半硅氧烷,英文名称polyhedral oligomericsilsesquioxane,简称POSS,通式(RSiO3/2)n,其中R为八个顶角Si原子所连接基团。本发明中,单乙烯基笼型聚倍半硅氧烷,即七个顶角连接有含溴端基,还有一个顶角为端乙烯基;进一步,通过端乙烯基与氯乙烯、丙烯酸酯进行共聚反应,得到改性PVC材料的主体成分,而含溴端基则继续在催化剂作用下,与多元胺进行反应实现离子化,然后与含阴离子盐进行离子交换得到含离子液体笼型聚倍半硅氧烷改性的PVC聚合物。含离子液体笼型聚倍半硅氧烷改性的PVC聚合物,不仅可实现POSS与离子液体的协同阻燃作用,而且离子液体具有良好的导电性,提高了改性PVC光缆料的防静电性能,而接枝的POSS基团,由于POSS基团的笼型结合特性,则进一步提高了改性PVC光缆料的抗冲击性能和低温脆性性能。
进一步地,所述乳化剂为十二烷基硫酸钠、十二烷基苯磺酸钠、油酸钾、硬脂酸钾中的至少一种。
进一步地,所述交联剂为乙二醇二丙烯酸酯、1,3-丙烷二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,5-戊二醇二丙烯酸酯中的至少一种。本发明的交联剂,不仅进一步提高了PVC光缆料的抗冲击性,而且使得PVC光缆料的塑化时间缩短,熔融温度降低,加工扭矩明显降低,易于加工。
进一步地,所述引发剂为过硫酸钾、过硫酸铵、过硫酸钠中的至少一种。
进一步地,所述多元胺为四甲基乙二胺、四甲基丁二胺、三亚乙基二胺中的至少一种。
进一步地,所述催化剂为碘化钠和/或碘化钾。
进一步地,所述含阴离子盐为四氟硼酸钠和/或六氟磷酸钾。
进一步地,所述硅烷偶联剂为A151、A171、A172中的至少一种,所述纳米无机填料为磷酸钙、磷酸钾、磷酸铝中的至少一种,所述加工助剂为PVC401助剂,所述润滑剂为石蜡、硬脂酸钙、硬脂酸锌、硬脂酸钡、硬脂酸中的至少一种。磷酸盐纳米无机填料的添加,不仅增加了改性PVC光缆料的强度,而且提高了其阻燃性能。
相应地,采用如上述制备方法制备得到抗静电高阻燃PVC光缆料。
本发明的有益效果:
本发明采用以氯乙烯和单乙烯基笼型聚倍半硅氧烷作为反应单体,在引发剂的作用下,与交联剂进行交联聚合改性反应,改性后的PVC光缆料具有优异的抗冲击性能和耐低温脆性性能;通过接枝在侧链上的含离子液体笼型聚倍半硅氧烷的改性处理,不仅提高了PVC光缆料的防静电和阻燃性能,而且进一步提高了光缆料的抗冲击性能和耐低温脆性性能,从而使其满足石化、煤矿井下等严苛恶劣环境条件下的使用要求。
具体实施方式
以下描述用于揭露本发明以使本领域技术人员能够实现本发明。以下描述中的优选实施例只作为举例,本领域技术人员可以想到其他显而易见的变型。
实施例1
本实施例的抗静电高阻燃PVC光缆料的制备方法,其包括以下步骤:
S1:按质量比为1:2:0.03:0.01称取原料共聚单体、去离子水、十二烷基硫酸钠和乙二醇二丙烯酸酯,所述共聚单体为氯乙烯和单乙烯基笼型聚倍半硅氧烷,加入适量的过硫酸钾(约占上述混合物的0.01wt%),加热至30℃进行反应,反应结束后,真空抽滤,干燥,得到改性PVC预聚体;所述氯乙烯和单乙烯基笼型聚倍半硅氧烷的摩尔比为10:1;
S2:按重量份计,称取20份改性PVC预聚体溶于100份甲苯中,加入7.6份四甲基乙二胺和0.1份碘化钠,在60℃下搅拌反应2h,反应结束,抽滤得到固体产物;称取40份固体产物溶于100份乙腈中,再加入5份四氟硼酸钠,在25℃搅拌反应15h,反应结束后,将所得反应液倒入乙醇中析出沉淀物,所得混合液抽滤、滤饼真空干燥后制得含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;
S3:按重量份计,称取50份含离子液体笼型聚倍半硅氧烷改性的PVC聚合物、0.5份硅烷偶联剂A151、2份纳米无机填料磷酸钙、10份加工助剂PVC401助剂和5份润滑剂石蜡预混后,通过165℃温度挤塑后得到抗静电高阻燃PVC光缆料。
所述单乙烯基笼型聚倍半硅氧烷如化学式I所示
式中,R1为溴丙基,R2为烯丙基。
所述单乙烯基笼型聚倍半硅氧烷的制备方法包括以下步骤:在质量浓度为30%的丙酮的水溶液中,加入10份3-溴丙基三甲氧基硅烷和0.5份氢氧化钠进行水解,制备得到笼型聚倍半硅氧烷中间体,然后加入质量浓度为20%的烯丙基三甲氧基硅烷的三乙胺溶液,所述烯丙基三甲氧基硅烷与笼型聚倍半硅氧烷中间体的摩尔比为1:1,进行关环反应,得到单乙烯基笼型聚倍半硅氧烷。
实施例2
本实施例的抗静电高阻燃PVC光缆料的制备方法,其包括以下步骤:
S1:按质量比为1:2.5:0.04:0.03称取原料共聚单体、去离子水、十二烷基苯磺酸钠和1,4-丁二醇二丙烯酸酯,所述共聚单体为氯乙烯和单乙烯基笼型聚倍半硅氧烷,加入适量的过硫酸铵(约占上述混合物的0.01wt%),加热至40℃进行反应,反应结束后,真空抽滤,干燥,得到改性PVC预聚体;所述氯乙烯和单乙烯基笼型聚倍半硅氧烷的摩尔比为20:3;所述单乙烯基笼型聚倍半硅氧烷化学结构式同实施例1所示;
S2:按重量份计,称取30份改性PVC预聚体溶于100份甲苯中,加入11.5份四甲基丁二胺和0.3份碘化钠,在70℃下搅拌反应2h,反应结束,抽滤得到固体产物;称取50份固体产物溶于100份乙腈中,再加入7份四氟硼酸钠,在30℃搅拌反应24h,反应结束后,将所得反应液倒入乙醇中析出沉淀物,所得混合液抽滤、滤饼真空干燥后制得含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;
S3:按重量份计,称取80份含离子液体笼型聚倍半硅氧烷改性的PVC聚合物、1.5份硅烷偶联剂A171、5份纳米无机填料磷酸钾、12份加工助剂PVC401助剂和8份润滑剂硬脂酸锌预混后,通过175℃温度挤塑后得到抗静电高阻燃PVC光缆料。
实施例3
本实施例的抗静电高阻燃PVC光缆料的制备方法,其包括以下步骤:
S1:按质量比为1:3:0.05:0.05称取原料共聚单体、去离子水、硬脂酸钾和1,5-戊二醇二丙烯酸酯,所述共聚单体为氯乙烯和单乙烯基笼型聚倍半硅氧烷,加入适量的过硫酸钠(约占上述混合物的0.01wt%),加热至50℃进行反应,反应结束后,真空抽滤,干燥,得到改性PVC预聚体;所述氯乙烯和单乙烯基笼型聚倍半硅氧烷的摩尔比为30:5;所述单乙烯基笼型聚倍半硅氧烷化学结构式同实施例1所示;
S2:按重量份计,称取50份改性PVC预聚体溶于100份甲苯中,加入16.8份四三亚乙基二胺和0.5份碘化钾,在80℃下搅拌反应2h,反应结束,抽滤得到固体产物;称取60份固体产物溶于100份乙腈中,再加入12份六氟磷酸钾,在30℃搅拌反应24h,反应结束后,将所得反应液倒入乙醇中析出沉淀物,所得混合液抽滤、滤饼真空干燥后制得含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;
S3:按重量份计,称取100份含离子液体笼型聚倍半硅氧烷改性的PVC聚合物、2.5份硅烷偶联剂A172、8份纳米无机填料磷酸铝、15份加工助剂PVC401助剂和12份润滑剂硬脂酸预混后,通过185℃温度挤塑后得到抗静电高阻燃PVC光缆料。
对比例1
本对比例的抗静电高阻燃PVC光缆料的制备方法,其步骤与实施例1基本相似,不同之处在于,省略步骤S2。
对比例2
本对比例的抗静电高阻燃PVC光缆料的制备方法,其步骤与实施例1基本相似,不同之处在于,省略步骤S2,且步骤S1中改性PVC预聚体所采用的共聚单体仅为氯乙烯,未添加单乙烯基笼型聚倍半硅氧烷。
将实施例1~3和对比例1~2制备得到的改性PVC光缆料进行性能测试,其性能结果如表1所示:
其中,拉伸强度按GB/T1040.2-2006测试;弯曲弹性模量按GB/T 9341-2008测试;冲击强度按GB/T1043.2-2018测试;阻燃性能按GB/T 2406.2-2009(极限氧指数法)测试。
表1
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是本发明的原理,在不脱离本发明精神和范围的前提下本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明的范围内。
Claims (8)
1.一种抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述制备方法包括以下步骤:
S1:按质量比为1:2~3:0.03~0.05:0.01~0.05称取原料共聚单体、去离子水、乳化剂和交联剂,所述共聚单体为氯乙烯和单乙烯基笼型聚倍半硅氧烷,加入适量的引发剂,加热至30~50℃进行反应,反应结束后,真空抽滤,干燥,得到改性PVC预聚体;
S2:按重量份计,称取20~50份改性PVC预聚体溶于100份甲苯中,加入7.6~16.8份多元胺和0.1~0.5份催化剂,在60~80℃下搅拌反应1~2h,反应结束,抽滤得到固体产物;称取40~60份固体产物溶于100份乙腈中,再加入3~12份含阴离子盐,在20~30℃搅拌反应15~24h,反应结束后,将所得反应液倒入乙醇中析出沉淀物,所得混合液抽滤、滤饼真空干燥后制得含离子液体笼型聚倍半硅氧烷改性的PVC聚合物;
S3:按重量份计,称取50~100份含离子液体笼型聚倍半硅氧烷改性的PVC聚合物、0.5~2.5份硅烷偶联剂、2~8份纳米无机填料、10~15份加工助剂和5~12份润滑剂预混后,通过165~185℃温度挤塑后得到抗静电高阻燃PVC光缆料;
所述含阴离子盐为四氟硼酸钠和/或六氟磷酸钾;所述单乙烯基笼型聚倍半硅氧烷如化学式I所示
;
式中,R1为溴丙基或溴丁基,R2为乙烯基、烯丙基或己烯基。
2.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述乳化剂为十二烷基硫酸钠、十二烷基苯磺酸钠、油酸钾、硬脂酸钾中的至少一种。
3.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述交联剂为乙二醇二丙烯酸酯、1,3-丙烷二醇二丙烯酸酯、1,4-丁二醇二丙烯酸酯、1,5-戊二醇二丙烯酸酯中的至少一种。
4.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述引发剂为过硫酸钾、过硫酸铵、过硫酸钠中的至少一种。
5.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述多元胺为四甲基乙二胺、四甲基丁二胺、三亚乙基二胺中的至少一种。
6.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述催化剂为碘化钠和/或碘化钾。
7.如权利要求1所述的抗静电高阻燃PVC光缆料的制备方法,其特征在于,所述硅烷偶联剂为A151、A171、A172中的至少一种,所述纳米无机填料为磷酸钙、磷酸钾、磷酸铝中的至少一种,所述加工助剂为PVC401助剂,所述润滑剂为石蜡、硬脂酸钙、硬脂酸锌、硬脂酸钡、硬脂酸中的至少一种。
8.一种抗静电高阻燃PVC光缆料,其特征在于,所述PVC光缆料采用如权利要求1-7任一项所述制备方法制备得到。
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