CN104672603A - 一种纳米阻燃电缆材料的制备方法 - Google Patents
一种纳米阻燃电缆材料的制备方法 Download PDFInfo
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- CN104672603A CN104672603A CN201510145584.6A CN201510145584A CN104672603A CN 104672603 A CN104672603 A CN 104672603A CN 201510145584 A CN201510145584 A CN 201510145584A CN 104672603 A CN104672603 A CN 104672603A
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- UAMZXLIURMNTHD-UHFFFAOYSA-N dialuminum;magnesium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Mg+2].[Al+3].[Al+3] UAMZXLIURMNTHD-UHFFFAOYSA-N 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
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Abstract
本发明公开了一种纳米阻燃电缆材料的制备方法,所述纳米阻燃电缆材料的制备原料包括:改性水滑石10-30份,防老剂1-3.5份,促进剂1-2.8份,增塑剂0.6-1.5份,纳米活性剂5-12份。本发明使用的防老剂为:6-乙氧基-2,2,4-三甲基-1,2-二氢化喹啉,其商品名称为防老剂AW。防老剂AW为褐色粘稠液体,纯品为浅褐色粘筒液体。无毒,比重为1.029~1.030(25℃),沸点为169℃。能溶于苯、丙酮、二氧乙烷、四氯化碳、溶剂汽油和乙醇;不溶于水。贮存稳定。是特效的防臭氧防老剂、对屈挠龟裂和热氧老化亦有防护作用。本发明改性阻燃EVA的力学性能、阻燃性能、耐热性能都较好。
Description
技术领域
本发明涉及电缆材料技术领域,特别涉及一种纳米阻燃电缆材料的制备方法。
背景技术
随着计算机及网络工程的不断发展,出于对机房安全的考虑,人们越来越多地使用无卤阻燃电缆和硅烷交联电缆。由于EVA树脂具有良好的填料包容性和可交联性,因此在无卤阻燃电缆、半导体屏蔽电缆和二步法硅烷交联电缆中使用较多。另外,EVA树脂还被应用于制作一些特殊电缆的护套。在电线电缆中使用的EVA树脂,醋酸乙烯含量一般在12%~24%。
阻燃剂的分类可根据元素种类分为卤系、有机磷系、及卤磷系、硅系、铝镁系、钼系、硼系、氮系等。卤系阻燃剂长期以来以其阻燃效率高、用量少、价格低而闻名于世。自从1986年欧洲首先发现含溴体系燃烧产生的产物中含有的多溴二苯醚、四溴双苯并二恶烷及四溴双苯并呋喃等属于致癌物质,含卤阻燃体系一统天下的局面已经受到了严峻的挑战,采用无卤阻燃材料与产品已是大势所趋的事实。欧盟两项指令“废弃电子电器设备指令”(WEEE)及“电子电器设备中禁用有害物质指令”(RoHS)的颁布加速了这一进程。无机阻燃剂(硼系,硅系等)虽然具有低毒,抗腐烛性,价廉,燃烧过程中低烟等优点,但是却有一些非常严重的缺点,如低的阻燃效率和热稳定性,对材料的物理机械性能造成较大程度的恶化。近年来人们致力于环境友好型阻燃剂的研究与开发,其热点主要集中在化学膨胀阻燃体系和纳米阻燃体系。
Eva:乙烯-醋酸乙烯共聚物,英文简称:EVA,编码:1314,分子式:(C2H4)x.(C4H6O2)y,化学性质:通用高分子聚合物。乙烯与醋酸乙烯共聚物是乙烯共聚物中最重要的产品,国外一般将其统称为EVA。但是在我国,人们根据其中醋酸乙烯含量的不同,将乙烯与醋酸乙烯共聚物分为EVA树脂、EVA橡胶和VAE乳液。醋酸乙烯含量小于40%的产品为EVA树脂;醋酸乙烯含量40%~70%的产品很柔韧;富有弹性特征,人们将这一含量范围的EVA树脂有时称为EVA橡胶;醋酸乙烯含量在70%~95%范围内通常呈乳液状态,称为VAE乳液。
EVA中的醋酸乙烯的含量低于20%时,这时才可作为塑料使用。EVA有很好的耐低温性能,其热分解温度较低,约为230℃左右,随着分子量的增大,EVA的软化点上升,加工性和塑件表面光泽性下降,但强度增加,冲击韧性和耐环境应力开裂性提高,EVA的耐化学药品、耐油性方面较之PE,PVC稍差,并随醋酸乙烯含量的增加,变化更加明显。
EVA树脂是乙烯-醋酸乙烯共聚物,一般醋酸乙烯(VA)含量在5%~40%。与聚乙烯相比,EVA由于在分子链中引入了醋酸乙烯单体,从而降低了高结晶度,提高了柔韧性、抗冲击性、填料相溶性和热密封性能,被广泛应用于发泡鞋料、功能性棚膜、包装膜、热熔胶、电线电缆及玩具等领域。一般来说,EVA树脂的性能主要取决于分子链上醋酸乙烯的含量。
化学膨胀型阻燃(intμmescent flame retardant)体系起源于传统的所谓“三源”:即酸源、炭源、气源三个基本组分构成的一类阻燃体系。化学膨胀型阻燃技术起源于20世纪30年代出现的膨胀型防火涂料。Tramm于1938年提出了第一篇关于膨胀型防火涂料的专利Tramm在专利中指出,在基材表面的这种防火涂料在加热的时候可以形成膨胀的炭层,从而能够有效地保护基材免受火焰的进一步燃烧。之后Olsen和Bechle在1948年使用了“膨胀”一词描述聚合物受热或燃烧时所发生的膨胀或发泡现象。Jones等详细研究了膨胀限燃体系多种成分所起的作用,将提供炭的碳化物称之为炭源,而将导致泡珠效应的化合物称之为发泡源。另外在燃烧时生成酸的称之为酸源。在化学膨胀型阻燃技术应用于聚合物研究的初期,即20世纪70年代至80年代间,Camino等为推进这一技术的研究与发展,围绕化学膨胀型阻燃体系在聚稀烃中的应用,开展了一系列的基础研究。其中最为典型的是聚磷酸铵/季戊四醇(APP/PER)阻燃聚丙稀(PP)为基础的阻燃体系。
尽管目前膨胀型阻燃剂的合成报道很多,但是大多数仍处于实验室的研究阶段,并没有实现工业化生产,主要原因如下:(1)膨胀型阻燃剂吸湿性强。比如,以APP/MEL/PER为主要成分的膨胀型阻燃剂,各个组分之间较易发生醇解,使得阻燃的基体抗水性下降。(2)膨胀型阻燃剂与基体的相容性差,使得基体的绝缘性能和电性能下降,尤其是力学性能如抗冲击强度和拉伸强度都会大幅度下降。(3)膨胀型阻燃刻的相对分子量都较小,比较容易迁移到聚合物的表面,也会使材料的热稳定性下降,最终导致基体的物理机械性能和外观性下降。(4)膨胀型阻燃剂与基体之间的理论配比仍不明确。(5)膨胀型阻燃剂的添加量仍需较大。
协同阻燃是指由两种或者两种以上的组分构成的阻燃体系,其阻燃效果优于各组分阻燃效果之和到目前为止,典型的协同阻燃体系主要包括卤磷协同、卤祶协同、磷氮协同等。纳米材料自20世纪80年代开.发问世之后,引起了世界各国的极大关注,而研究表明纳米阻燃剂在低添加量下就可以使系统的热释放速率(HRR)和热释放速率峰值(PHRR)有明显的降低。由于卤系阻燃刻对环境的危害,膨胀阻燃剂与纳米阻燃剂受到越来越多的关注,而膨胀阻燃与纳米技术的结合,添加MMT、LDH、CNT、POSS等,在提高阻燃效率的同时,又能不同程度地改善阻燃聚合物材料的热稳定性、物理机械性能等。所以,对这两者之间的协同研究也最为集中。
膨胀/纳米协同阻燃具有代表性的是关于分子筛应用于APP/PER体系的研究。研究发现1%~1.5%含量的分子筛可以使添加30%APP/PER的膨胀型阻燃PP、PE、PS以及乙稀基聚合物的LOI提高了2~20。
在聚合物纳米复合物材料与膨胀阻燃结合的研究中,应用最多的是MMT。这与MMT来源丰富、纳米片层结构较易在聚合物链中插层等有关,也与层状桂酸盐对膨胀阻燃体系热降解成炭过程中的催化作用有关。数据表明,MMT纳米复合物体系的加入导致膨胀阻燃PP的HRR普遍下降。研究指出MMT与IFR之间的协同作用机理是降解反应产生的酸性点具有强烈的催化作用,有利于膨胀阻燃体系氧化脱氢交联成炭过程的进行;在燃烧过程中,纳米复合物表面重组形成耐热的硅酸盐炭层,加强了炭层对氧及挥发产物的阻隔作用。
碳纳米管的加入对聚合物的抗热与阻燃性能都能带来正面效果,所以它与膨胀阻燃剂的结合,能够达到改善聚合物成炭质量、提高阻燃性能,同时改善热稳定性和力学等性能。
尽管纳米/膨胀协同阻燃体系的研究有了很大的进步,但仍有很多问题虽待解决:(1)膨胀型阻燃剂与纳米阻燃剂的协同目前仍旧停留在将两者直接共混的阶段,因此协同效果仍有较大提高空间;(2)膨胀/纳米协同阻燃的机理仍不清楚,如硅酸盐与膨胀型阻燃及各组分的相互反应、残炭结构的定量表征、硅酸盐对膨胀型阻燃剖及聚合物基体的催化作用仍然很笼统;(3)膨胀/纳米协同阻燃体系是一个复杂的多相体系,多元组分共存时对彼此微观结构的影响以及对复合体系最终阻燃性能的关系仍需进一步的研究。
由于EVA与无机填料的相容性好,所以,现有技术中EVA的阻燃一般采用填充量较大且具有一定抑烟作用的无机填料阻燃剂阻燃。氢氧化镁(MH)和氢氧化铝(ATH)是EVA比较适合的阻燃剂,但是ATH的阻燃效果不及MH。研究表明,MH对EVA有促进成炭的作用,而且其填充的EVA残留物热稳定性更高。但锥形量热的数据表明,在高添加量(49%)的情况下,ATH比MH更有效,但MH能够延长点燃时间,而ATH不行,且在低添加量时点燃时间甚至缩短。
现有技术中,含卤阻燃剂体系对EVA也有较好的阻燃效果,十溴二苯醚与三氧化二锑并用能够获得较好的阻燃效果,但是由于溴系阻燃剂会产生有毒气体及浓烟的缺点,其在电线电缆阻燃材料中应用的也不多。
发明内容
本发明所要解决的技术问题在于,提供了一种纳米阻燃电缆材料及其制备应用。本发明纳米协同改性阻燃EVA的力学性能、阻燃性能、耐热性能都较好。
为解决上述技术问题,本发明提供了一种纳米协同改性阻燃EVA电缆材料。
改性水滑石LDHs的制备
将一定量的镁铝水滑石分散于脱CO2的去离子水中制成浆液后将过量的NaH2PO4·2H2O溶于水所配成溶液缓慢倒入浆液中,加热搅拌并用稀硝酸调节PH至4.5左右,回流温度下反应1.5小时。待自然冷却后,用脱CO2的去离子水洗涤产物并过滤直至滤液PH=7,然后干燥得到LDHs。
改性水滑石M-LDHs的制备
取适量的碳酸根插层镁铝水滑石(LDHs)于三口烧瓶中,并加入适量脱CO2的去离子水后分散于三口烧瓶中形成良好的浆液。将适量NaH2PO4·2H2O溶于水中配成溶液,然后将所配溶液缓慢倒入浆液中,并不停加热搅拌,并用稀HNO3调节PH值至4-5左右,然后升温至100℃-105℃反应,回流温度下反应2.5h后自然冷却。并用脱除CO2的去离子水洗涤产物并过滤直至滤液的PH=7,然后在60℃下于鼓风干燥箱中干燥6h后得到产物MgAl-H2PO4-LDHs(M-LDHs)。
如图1所示,为本发明实施例中给出得两种水滑石(LDHs和M-LDHs)的TEM照片,可以看出LDHs为明显的类六边形,M-LDHs为近圆形的片层状材料,改性前后LDHs和M-LDHs两者的形貌有变化,片层表面的尺寸大概为50-150nm。
本发明使用的防老剂可以为:6-乙氧基-2,2,4-三甲基-1,2-二氢化喹啉。其商品名称为防老剂AW。防老剂AW为褐色粘稠液体,纯品为浅褐色粘筒液体。无毒,比重为1.029~1.030(25℃),沸点为169℃。能溶于苯、丙酮、二氧乙烷、四氯化碳、溶剂汽油和乙醇;不溶于水。贮存稳定。是特效的防臭氧防老剂、对屈挠龟裂和热氧老化亦有防护作用。特别适用于动态条件下使用的制品。
本发明使用的防老剂还可以为:2,2,4-三甲基1,2-二氢化喹聚合体。商品名称为防老剂RD。防老剂RD为琥珀至灰白色树脂状粉末,无毒。软化点不低于74℃。能溶于丙酮、苯、氯仿、二硫化碳、微溶于石油烃;不溶于水。能抑制条件较苛刻的氧化,热老化及天候老化作用,但对屈挠龟裂防护效果较差。不喷霜、有轻微污染性。一般用量范围为0.5~2份,最高可达3成份。
本发明的防老剂又可以为:N-苯基-α-苯胺。商品名称为防老剂A。防老剂A为黄褐色至紫色结晶状物质,纯品为无色片状结晶,因含少量甲萘胺及苯胺,有毒,不可与皮肤接触。比重为1.16~1.17,熔点不低于52.0℃。易溶于丙酮、乙酸乙酯、苯、乙醇、氯仿、四氯化碳;可溶于汽油;不溶于水。日光及空气中渐变紫色。易燃。防老剂A对热、氧、屈挠及天候等老化作用均有良好的防护效果,为天然橡胶、合成橡胶及再生胶的通用防老剂。在氯丁橡胶中兼有抗臭氧老化的性能;对变价金属离子的老化作用及再生胶亦有一定的抑制效果在干胶中易分散,亦易分散于水中;在橡胶中的溶解度高达5%,比防老剂D大,用量在3~4份时不喷霜,故可增加用量以提高防护效能。
本发明防老剂也可以为:N-苯基-β-萘胺。商品名称为防老剂D。防老剂D为浅灰色至浅棕色粉末,纯品为白色粉末。比重为1.18,熔点不低于104℃。易溶剂于丙酮、乙酸乙酯、二硫化碳、氯仿;可溶于乙醇、四氯化碳;不溶于汽油和水。在空气及日光下逐渐变为灰黑色,但不影响防护效果。易燃。防老剂D为天然橡胶、合成橡胶及胶乳的通用型防老剂。对热、氧、屈挠龟裂及一般老化因素均有良好的防护作用,并稍优于防老剂A。对有害金属的离子亦有防护作用,但较防老剂A差。若与防老剂4040或4010NA并用,抗热、氧、屈挠龟裂以及抗臭氧老化性能均有显著增加。在干胶中易分散于水中。
本发明实施例使用的促进剂为下述产品中的一种或多种:促进剂T、促进剂DM、促进剂BZ。
本发明增塑剂可以为:邻苯二甲酸二辛脂(DOP)。增塑剂DOP为无色油状液体,比重0.9861(20/20),熔点-55,沸点370(常压),不溶于水,溶于乙醇、乙醚、矿物油等大多数有机溶剂。通用级DOP,广泛用于塑料、橡胶、油漆及乳化剂等工业中。DOP是通用型增塑剂,主要用于聚氯乙烯脂的加工、还可用于化地树脂、醋酸树脂、ABS树脂及橡胶等高聚物的加工,也可用于造漆、染料、分散剂等、DOP增塑的PVC可用于制造人造革、农用薄膜、包装材料、电缆等。
本发明增塑剂还可以为:多元醇苯甲酸酯。多元醇苯甲酸酯与聚氯乙稀和氯乙稀醋酸乙稀共聚物、聚醋酸乙稀有良好的相溶性,还和聚氯乙稀,聚甲基丙稀酸甲酯,聚乙稀醇缩丁醛,硝基纤维素,醋酸丁酯纤维素和乙基纤维素等相溶。多元醇苯甲酸酯色泽浅、增塑效率高、相溶性好、挥发性低、渗出性低、热稳定指标高、耐寒耐水抽出、不易氧化和挥发、电气性能优良、填充剂容量大,制品光亮度高等特点。广泛用于PVC塑料颗粒、非填充压延膜、人造革、电缆料、板材、片材、软硬管材、鞋底料、橡塑条、发泡料、薄膜、油漆、橡胶、有机玻璃、印刷油墨、增塑糊、醋酸乙烯乳液粘合剂等。是增塑剂行业售价最低的一种,可以大幅降低橡胶产品成本。
本发明增塑剂也可以为:己二酸二辛酯。其化学名为:己二酸二一2一乙基己酯,分子式为C22H42O4,己二酸二辛酯是无色无味透明油状液体,能溶于乙醇、乙醚、丙酮、醋酸等大多数有机溶剂,微溶于乙二醇,不溶于水。但己二酸二辛酯的挥发性大,耐水性、迁移性、绝缘性等方面有一定不足。己二酸二辛酯常与邻苯二甲酸酯类复配,应用于耐寒农用薄膜、电缆包覆层、人造革、板材、户外用水管及冷冻食品包装膜等。己二酸二辛酯还可以用作多种合成橡胶的低温用增塑剂以及硝基纤维素、乙基纤维素、聚苯乙烯、氯乙烯一醋酸丁烯共聚物等树脂的耐寒增塑剂。目前,己二酸二正己酯还大量应用于聚乙烯醇缩丁醛树脂胶片中。此外,在许多国家,法定其可用作食品、医药包装塑料的增塑剂。
本发明增塑剂又可以为:己二酸二正己酯。己二酸二正己酯是世界上用量最大的耐寒型增塑剂。己二酸正辛正癸酯,无色透明液体,是由己二酸与直链的正辛醇、正癸醇酯化合成的直链型脂肪二元酸混合酯;己二酸正辛正癸酯溶于矿物油、汽油和大多数有机溶剂,不溶或微溶于甘油、乙二醇类和某些胺类,是性能优良的直链型耐寒性增塑剂。与己二酸支链醇相比具有更好的耐低温性能,并且挥发损失、耐热性和耐光性、耐水抽出性等也较支链醇酯优良。当其与邻苯二甲酸酯共用时,能改进聚氯乙烯醋酸乙烯酯共聚物乳液性能,广泛地用于聚醋酸乙烯酯、聚苯乙烯、聚甲基丙烯酸甲酯、硝酸纤维素、乙基纤维素和橡胶的耐寒增塑剂。
本发明增塑剂在可以为:邻苯二甲酸丁苄酯(Butyl benzyl phthalate)分子量312.40。性质:无色透明油状液体。相对密度(25℃/4℃)1.116,凝固点-35℃,沸点370℃.闪点(开口)199℃.折射率1。535.粘度(25℃)41.5mPa·s,溶于有机溶剂和烃类。不溶于水。可燃。微毒。与大多数橡胶和树脂相容性良好.溶剂化作用强,用作耐水性耐热、耐油抽出性的增塑剂。
本发明增塑剂还可以为:耐寒增塑剂DOS。癸二酸二辛酯(DOS),学名:癸二酸二(2-乙基己)酯分子式:C26H50O4。耐寒增塑剂DOS为无色或淡黄色透明油状液体,凝固点-48℃,沸点:256℃(0.67Kpa),着火点257-263℃,黏度25mPa.s(20℃),折光率1.449-1.451(25℃),能溶于烃类、醇类、酮类、酯类、氯代烃类等有机溶剂,不溶于二元醇类及水。耐寒增塑剂DOS为一种聚氯乙烯优良的耐寒增塑剂,增塑效率高,挥发性低,因此除具有优良的低温耐寒性能外,又有较好的耐热性,可在较高的温度下使用。本品的耐候性较好,电气绝缘性能也较优,常与邻苯二甲酸酯类并用,特别适用于耐寒电线和电缆料、人造革、薄膜、板材、片材等制品。耐寒增塑剂DOS可以用作多种合成橡胶的低温用增塑剂以及硝基纤维素、乙基纤维素、聚甲基丙烯酸甲酯、聚苯乙烯、氯乙烯共聚物等树脂的耐寒增塑剂。
制备原料中包括的纳米活性剂为下列化合物(或混合物)中的一种或多种:MgO、Al2O3、Si3N4、BN、高纯度碳粉、AlN、ZnO、KAl(SO4)2·12H2O(明矾)、Al2O3-2SiO2-2H2O(高岭土)。
本发明实施例使用的MgO为纳米MgO颗粒。
本实施例采用室温固相法制备MgO颗粒。
本实施例室温固相法制备MgO颗粒的具体方法优选为:将MgCI溶液与Na2CO3(原料质量配比1∶1.2)溶液,以PVA溶液(聚乙烯醇溶液)为改性剂,反应产生沉淀MgCO3沉淀,然后在75~85℃恒温下,通过沉淀转化的方式得到了碱式碳式镁前驱体。50~60℃静置碱式碳式镁前驱体沉淀24-30小时。最后在Ar气流通入,温度为600~650℃的条件下锻烧,得到了纳米MgO颗粒。采用PVA作为高分子表面活性剂,控制了颗粒的团聚,所制得的纳米MgO颗粒分散性较好,为立方结构,基本呈球形,其粒径为25-35nm。
本发明有益的技术效果在于:本发明纳米协同改性阻燃EVA的力学性能、阻燃性能、耐热性能都较好。
附图说明
图1为本发明实施例所述了两种水滑石(LDHs和M-LDHs)的TEM照片;
图2为本发明实施例所述试验材料在400℃马弗炉中加热燃烧30min后的数码相片;
图3为本发明实施例所述未经过任何表面处理的氢氧化镁的应力应变曲线。
具体实施方式
以下将结合实施例来详细说明本发明的实施方式,借此对本发明如何应用技术手段来解决技术问题,并达成技术效果的实现过程能充分理解并据以实施。
本发明实施例原料:
EVA(360)1000份:美国杜邦,熔体流动速率为2g/10min,密度为0.948g/cm3,自制改性水滑石10-30份,防老剂1-4份,促进剂1-3份,增塑剂0.6-1.5份,纳米活性剂5-11份。
改性水滑石LDHs的制备方法
将镁铝水滑石分散于脱CO2的去离子水中制成浆液后,将NaH2PO4·2H2O溶于水配成过饱和溶液缓慢倒入浆液中,加热搅拌并用稀硝酸调节PH至4.2~4.3,回流温度下反应1.5小时。待自然冷却后,用脱CO2的去离子水洗涤产物并过滤直至滤液PH=7,然后干燥得到碳酸根插层镁铝水滑石(LDHs)。
改性水滑石M-LDHs的制备方法
取碳酸根插层镁铝水滑石(LDHs)于三口烧瓶中,并加入脱CO2的去离子水后分散于三口烧瓶中形成良好的浆液。将NaH2PO4·2H2O溶于水中配成饱和溶液,然后将所配溶液缓慢倒入浆液中,并不停加热搅拌,并用稀HNO3调节PH值至4.8~5.0,然后升温至100℃-105℃反应,回流温度下反应2.5h后自然冷却。并用脱除CO2的去离子水洗涤产物并过滤直至滤液的PH=7,然后在60℃下于鼓风干燥箱中干燥6h后得到产物MgAl-H2PO4-LDHs(M-LDHs)。
如图1所示,为本发明实施例中给出得两种水滑石(LDHs和M-LDHs)的TEM照片,可以看出LDHs为明显的类六边形,M-LDHs为近圆形的片层状材料,改性前后LDHs和M-LDHs两者的形貌有一定的变化,片层表面的尺寸大概为50-150nm。
本发明一实施例使用的防老剂为:6-乙氧基-2,2,4-三甲基-1,2-二氢化喹啉,其商品名称为防老剂AW。防老剂AW为褐色粘稠液体,纯品为浅褐色粘筒液体。无毒,比重为1.029~1.030(25℃),沸点为169℃。能溶于苯、丙酮、二氧乙烷、四氯化碳、溶剂汽油和乙醇;不溶于水。贮存稳定。是特效的防臭氧防老剂、对屈挠龟裂和热氧老化亦有防护作用。特别适用于动态条件下使用的制品。
本发明另一实施例使用的防老剂为:2,2,4-三甲基1,2-二氢化喹聚合体。商品名称为防老剂RD。防老剂RD为琥珀至灰白色树脂状粉末,无毒。软化点不低于74℃。能溶于丙酮、苯、氯仿、二硫化碳、微溶于石油烃;不溶于水。能抑制条件较苛刻的氧化,热老化及天候老化作用,但对屈挠龟裂防护效果较差。不喷霜、有轻微污染性。一般用量范围为0.5~2份,最高可达3成份。
本发明再一实施例使用的防老剂为:N-苯基-α-苯胺。商品名称为防老剂A。防老剂A为黄褐色至紫色结晶状物质,纯品为无色片状结晶,因含少量甲萘胺及苯胺,有毒,不可与皮肤接触。比重为1.16~1.17,熔点不低于52.0℃。易溶于丙酮、乙酸乙酯、苯、乙醇、氯仿、四氯化碳;可溶于汽油;不溶于水。日光及空气中渐变紫色。易燃。防老剂A对热、氧、屈挠及天候等老化作用均有良好的防护效果,为天然橡胶、合成橡胶及再生胶的通用防老剂。在氯丁橡胶中兼有抗臭氧老化的性能;对变价金属离子的老化作用及再生胶亦有一定的抑制效果在干胶中易分散,亦易分散于水中;在橡胶中的溶解度高达5%,比防老剂D大,用量在3~4份时不喷霜,故可增加用量以提高防护效能。
本发明又一实施例使用的防老剂为:N-苯基-β-萘胺。商品名称为防老剂D。防老剂D为浅灰色至浅棕色粉末,纯品为白色粉末。比重为1.18,熔点不低于104℃。易溶剂于丙酮、乙酸乙酯、二硫化碳、氯仿;可溶于乙醇、四氯化碳;不溶于汽油和水。在空气及日光下逐渐变为灰黑色,但不影响防护效果。易燃。防老剂D为天然橡胶、合成橡胶及胶乳的通用型防老剂。对热、氧、屈挠龟裂及一般老化因素均有良好的防护作用,并稍优于防老剂A。对有害金属的离子亦有防护作用,但较防老剂A差。若与防老剂4040或4010NA并用,抗热、氧、屈挠龟裂以及抗臭氧老化性能均有显著增加。在干胶中易分散于水中。
本发明实施例使用的促进剂为下述产品中的一种或多种:促进剂T、促进剂DM、促进剂BZ。
本发明一实施例使用的增塑剂为:邻苯二甲酸二辛脂(DOP)。增塑剂DOP为无色油状液体,比重0.9861(20/20),熔点-55,沸点370(常压),不溶于水,溶于乙醇、乙醚、矿物油等大多数有机溶剂。通用级DOP,广泛用于塑料、橡胶、油漆及乳化剂等工业中。DOP是通用型增塑剂,主要用于聚氯乙烯脂的加工、还可用于化地树脂、醋酸树脂、ABS树脂及橡胶等高聚物的加工,也可用于造漆、染料、分散剂等、DOP增塑的PVC可用于制造人造革、农用薄膜、包装材料、电缆等。
本发明另一实施例使用的增塑剂为:多元醇苯甲酸酯。多元醇苯甲酸酯与聚氯乙稀和氯乙稀醋酸乙稀共聚物、聚醋酸乙稀有良好的相溶性,还和聚氯乙稀,聚甲基丙稀酸甲酯,聚乙稀醇缩丁醛,硝基纤维素,醋酸丁酯纤维素和乙基纤维素等相溶。多元醇苯甲酸酯色泽浅、增塑效率高、相溶性好、挥发性低、渗出性低、热稳定指标高、耐寒耐水抽出、不易氧化和挥发、电气性能优良、填充剂容量大,制品光亮度高等特点。广泛用于PVC塑料颗粒、非填充压延膜、人造革、电缆料、板材、片材、软硬管材、鞋底料、橡塑条、发泡料、薄膜、油漆、橡胶、有机玻璃、印刷油墨、增塑糊、醋酸乙烯乳液粘合剂等。是增塑剂行业售价最低的一种,可以大幅降低橡胶产品成本。
本发明再一实施例使用的增塑剂为:己二酸二辛酯。其化学名为:己二酸二一2一乙基己酯,分子式为C22H42O4,己二酸二辛酯是无色无味透明油状液体,能溶于乙醇、乙醚、丙酮、醋酸等大多数有机溶剂,微溶于乙二醇,不溶于水。但己二酸二辛酯的挥发性大,耐水性、迁移性、绝缘性等方面有一定不足。己二酸二辛酯常与邻苯二甲酸酯类复配,应用于耐寒农用薄膜、电缆包覆层、人造革、板材、户外用水管及冷冻食品包装膜等。己二酸二辛酯还可以用作多种合成橡胶的低温用增塑剂以及硝基纤维素、乙基纤维素、聚苯乙烯、氯乙烯一醋酸丁烯共聚物等树脂的耐寒增塑剂。目前,己二酸二正己酯还大量应用于聚乙烯醇缩丁醛树脂胶片中。此外,在许多国家,法定其可用作食品、医药包装塑料的增塑剂。
本发明又一实施例使用的增塑剂为:己二酸二正己酯。己二酸二正己酯是世界上用量最大的耐寒型增塑剂。己二酸正辛正癸酯,无色透明液体,是由己二酸与直链的正辛醇、正癸醇酯化合成的直链型脂肪二元酸混合酯;己二酸正辛正癸酯溶于矿物油、汽油和大多数有机溶剂,不溶或微溶于甘油、乙二醇类和某些胺类,是性能优良的直链型耐寒性增塑剂。与己二酸支链醇相比具有更好的耐低温性能,并且挥发损失、耐热性和耐光性、耐水抽出性等也较支链醇酯优良。当其与邻苯二甲酸酯共用时,能改进聚氯乙烯醋酸乙烯酯共聚物乳液性能,广泛地用于聚醋酸乙烯酯、聚苯乙烯、聚甲基丙烯酸甲酯、硝酸纤维素、乙基纤维素和橡胶的耐寒增塑剂。
本发明又一实施例使用的增塑剂为:邻苯二甲酸丁苄酯(Butyl benzylphthalate)分子量312.40。性质:无色透明油状液体。相对密度(25℃/4℃)1.116,凝固点-35℃,沸点370℃.闪点(开口)199℃.折射率1。535.粘度(25℃)41.5mPa·s,溶于有机溶剂和烃类。不溶于水。可燃。微毒。与大多数橡胶和树脂相容性良好.溶剂化作用强,用作耐水性耐热、耐油抽出性的增塑剂。
本发明又一实施例使用的增塑剂为:耐寒增塑剂DOS。癸二酸二辛酯(DOS),学名:癸二酸二(2-乙基己)酯分子式:C26H50O4。耐寒增塑剂DOS为无色或淡黄色透明油状液体,凝固点-48℃,沸点:256℃(0.67Kpa),着火点257-263℃,黏度25mPa.s(20℃),折光率1.449-1.451(25℃),能溶于烃类、醇类、酮类、酯类、氯代烃类等有机溶剂,不溶于二元醇类及水。耐寒增塑剂DOS为一种聚氯乙烯优良的耐寒增塑剂,增塑效率高,挥发性低,因此除具有优良的低温耐寒性能外,又有较好的耐热性,可在较高的温度下使用。本品的耐候性较好,电气绝缘性能也较优,常与邻苯二甲酸酯类并用,特别适用于耐寒电线和电缆料、人造革、薄膜、板材、片材等制品。耐寒增塑剂DOS可以用作多种合成橡胶的低温用增塑剂以及硝基纤维素、乙基纤维素、聚甲基丙烯酸甲酯、聚苯乙烯、氯乙烯共聚物等树脂的耐寒增塑剂。
制备原料中包括的纳米活性剂为下列化合物(或混合物)中的一种或多种:MgO、Al2O3、Si3N4、BN、高纯度碳粉、AlN、ZnO、KAl(SO4)2·12H2O(明矾)、Al2O3-2SiO2-2H2O(高岭土)。
本发明实施例使用的MgO为纳米MgO颗粒。
纳米粉体材料工业化生产工艺要求制备方法简单,生产成本适宜,重复性好,粉体粒度均匀、产品纯度高、团聚程度低。现有技术中关于纳米氧化镁合成的方法很多,但实际上能够应用于工业生产的较少。一是因为设备、成本、原料、规模、投资等问题;二是有些工艺尚处于实验室研究阶段,实现工业化生产有困难,甚至有些根本不可能实现工业化生产。
本实施例采用室温固相法制备MgO颗粒。
本发明室温固相合成法克服了传统湿法制备氧化镁纳米颗粒存在的团聚问题,具有反应无需溶剂、产率高、反应条件易等优点;并克服了原有室温固相合成法中存在的效率低、粒子易氧化变形的缺点。
本实施例室温固相法制备MgO颗粒的具体方法为:将MgCI溶液与Na2CO3(原料质量配比1∶1.2)溶液,以PVA溶液(聚乙烯醇溶液)为改性剂,反应产生沉淀MgCO3沉淀,然后在75~85℃恒温下,通过沉淀转化的方式得到了碱式碳式镁前驱体。50~60℃静置碱式碳式镁前驱体沉淀24-30小时。最后在Ar气流通入,温度为600~650℃的条件下锻烧,得到了纳米MgO颗粒。采用PVA作为高分子表面活性剂,控制了颗粒的团聚,所制得的纳米MgO颗粒分散性较好,为立方结构,基本呈球形,其粒径为25-35nm。
本发明实施例使用的Si3N4为纳米氮化硅颗粒,满足下述指标:
本发明实施例使用的Si3N4还可以为高导热性氮化硅。普通的氮化硅具有无规取向的烧结结构。高导热性氮化硅是在原料粉体(粒径1μm以下)加入种晶粒子(直径1μm,长3-4μm),使这种种晶粒子取向排列,形成具有取向的长达100μm的纤维状氮化硅结构。由于纤维状结构的形成,导热系数呈现各相异性,在取向结构方向上导热系数为120w/(m·K),为普通氮化硅的3倍,相当于钢的导热系数。
本发明实施例使用的BN为纳米氮化硼颗粒,满足下述指标:
本发明实施例使用的高纯度碳粉为:东莞协力产的10000高纯碳粉。性能指标为:
固定碳: | 99.99% | 规格: | 10000目 |
牌号: | 18925457433 | 水分: | 0.015% |
膨胀度: | 1-2倍 | 筛上物粒度: | 0.0006% |
灰分: | 0.85 | 挥发分: | 0.01% |
筛下物粒度: | 0.0005% |
本发明实施例使用的AlN填料为:AlN晶须和AlN粒子做填料。本发明实施例中,将EVA作为基体,5μm以下AlN晶须和AlN粒子填充,获得高阻燃率的复合材料,AlN晶须和AlN粒子比率(质量比)是1∶20~30。本发明进一步研究了填料的混杂效应和偶联剂对复合材料阻燃率的影响。用适当比率的AlN晶须和AlN粒子混合,比单独用晶须和粒子赋予复合材料较高阻燃率。
本发明实施例使用的ZnO为:纳米氧化锌颗粒。其性能指标为:
本发明实施例使用的纳米氧化锌,为上述:1类纳米ZnO,2类纳米ZnO,3类纳米ZnO,中的一种。
Eva复合材料的制备
将EVA(360,美国杜邦实验)1000份在75℃下干燥8h后备用。在SHL-35型双螺杆挤出机中依次加入改性水滑石10-30份,防老剂1-3.5份,促进剂1-2.8份,增塑剂0.6-1.5份,纳米活性剂5-12份后挤出造粒,挤出温度设定依次为180℃、185℃、195℃、195℃、185℃,主机转速为40r/min。然后将干燥好的粒料在190℃下用平板硫化机压制成型并用万能制样机制得所需测试标准试样后,表征材料的阻燃性能、热性能及结晶性能等。
实验组表格:
性能测试和表征
极限氧指数(LOI)样品的LOI根据国标GB/T 2406-1993进行测试,具体样品尺寸为长70×6.5×3(±0.1)mm3,样品燃烧时间小于3min或燃烧长度小50mm时,以氧气体积分数表示的所需的氮氧气体的临界浓度即为材料的极限氧指数。
水平垂直燃烧等级(UL-94)
根据国标GB/T 2408-1996对PP复合材料进行垂直燃烧性能进行测试,样品尺寸为130×13×3mm3。每个样品至少测试5个试样,分级评估并记录材料的燃烧性能。
图2给出了试验材料在400℃马弗炉中加热燃烧30min后的数码相片;由图2中可以看出,纯Eva只有少量黑色残炭残留,且铺张面积极大;Eva/LDHs样品产生一个松散灰白的残炭结构,铺张面积与纯Eva相比减小;Eva/M-LDHs样品产生一个相对更紧致灰白的残炭结构,且铺张面积进一步减小。LDHs和M-LDHs在聚合物燃烧的过程中都能抑制其流延,M-LDHs形成的残炭面积更小,结构更致密,与LDHs相比,其具有更好的保护作用。
力学性能测试
将硫化成型的EVA复合材料放置在室温下3天后,在用制样机制成5B型哑铃状样条(遵循标准GB/T 1040-2006),以200mm/min的速度在万能材料试验机上做力学性能测试。
阻燃性能测试
将硫化成型的EVA复合材料放置在室温下3天后,按照国标GB/T2408.96分别切割成样条,在垂直燃烧仪上做阻燃性能测试。
垂直燃烧:UL.94(塑料)
HB:UL94标准中最底的阻燃等级。要求对于3到13毫米厚的样品,燃烧速度小于40毫米每分钟;小于3毫米厚的样品,燃烧速度小于70毫米每分钟;或者在100毫米的标志前熄灭。
V_2:对样品进行两次10秒的燃烧测试后,火焰在60秒内熄灭。可以有燃烧物掉下。
V-1:对样品进行两次10秒的燃烧测试后,火焰在60秒内熄灭。不能有燃烧物掉下。
V-0:对样品进行两次10秒的燃烧测试后,火焰在30秒内熄灭。不能有燃烧物掉下。
热性能
将硫化成型的EVA复合材料放置在室温下3天后,取适量在热分析仪上做热分解测试(TG),测试条件为纯氮气,升温速率为20摄氏度/分钟。并用纯Eva作为参考。
图3显示了未经过任何处理的纯Eva的应力应变曲线。我们可以从曲线中得出,从整个曲线的趋势看,应力随着Eva拉伸量的增长而增加。在伸长量0-2cm范围内,其应力几乎没有变化,而从2cm开始,其应力呈抛物线形式增长。在伸长量为14cm时,达到应力最大值140N。
下表显示了不同实验组对断裂拉伸强度与断裂伸长率的影响:
上表显示了不同实验组阻燃EVA对其断裂伸长率的变化的影响。很显然,各个实验组与纯Eva对照组之间的断裂拉伸强度与断裂伸长率差别明显。
将硫化成型的EVA复合材料放置在室温下3天后,按照国标GB/T2408-96分别切割成150×150x3mm样条,在垂直燃烧仪上做阻燃性能测试,结果如下:
上表列出了不同实验组阻燃EVA垂直燃烧的结果。对照组第一次平均燃烧时间为4s,在第二次燃烧时第36秒就产生熔滴,且平均时间36s,未达到阻燃级别;实验组I第一次平均燃烧时间为3s,但是第二次平均燃烧时间53S,阻燃性能稍差为V-2级别;实验组II第一次平均燃烧时间为2s,在第二次燃烧时间33S,阻燃级为V-1级别;实验组III其阻燃性能最好,两次平均燃烧时间总和只有3S,达到V-0级别;实验组IV第一次平均燃烧时间为2s,第二次平均燃烧时间为14s,阻燃级别达到V-0级别;实验组V第一次平均燃烧时间为3S,在第二次燃烧时间44S,阻燃级为V-1级别;实验组VI第一次平均燃烧时间为4s,但是第二次平均燃烧时间56S,为阻燃性能稍差为V-2级别。
上述结果说明本发明六组实验配方的阻燃剂协同阻燃,能够有效提高阻燃效率,减少阻燃剂用量和聚合物材料燃烧时的熔滴现象;而且能够在一定程度上提高阻燃材料的阻燃性能。
所有上述的首要实施这一知识产权,并没有设定限制其他形式的实施这种新产品和/或新方法。本领域技术人员将利用这一重要信息,上述内容修改,以实现类似的执行情况。但是,所有修改或改造基于本发明新产品属于保留的权利。
Claims (10)
1.一种纳米阻燃电缆材料的制备方法,其特征在于,所述纳米阻燃电缆材料的制备原料包括:EVA,改性水滑石,防老剂,促进剂,增塑剂,和,纳米活性剂。
2.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述EVA为美国杜邦360。
3.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述改性水滑石为LDHs。
4.根据权利要求3所述纳米阻燃电缆材料的制备方法,其特征在于,所述改性水滑石的制备方法包括:将镁铝水滑石分散于脱CO2的去离子水中制成浆液后,将NaH2PO4·2H2O溶于水配成过饱和溶液缓慢倒入浆液中,加热搅拌并用稀硝酸调节PH至4.2~4.3,回流温度下反应1.5小时;待自然冷却后,用脱CO2的去离子水洗涤产物并过滤直至滤液PH=7,然后干燥得到所述改性水滑石。
5.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述防老剂为:6-乙氧基-2,2,4-三甲基-1,2-二氢化喹啉。其商品名称为防老剂AW。
6.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述防老剂为:2,2,4-三甲基1,2-二氢化喹聚合体。
7.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述防老剂为:N-苯基-α-苯胺。
8.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述防老剂为防老剂D。
9.根据权利要求1所述纳米阻燃电缆材料的制备方法,其特征在于,所述促进剂为下述产品中的一种或多种:促进剂T、促进剂DM、促进剂BZ;所述增塑剂为:邻苯二甲酸二辛脂。
10.一种如权利要求1~9中任一项所述纳米阻燃电缆材料的制备方法制备的纳米阻燃电缆材料。
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CN105017661A (zh) * | 2015-06-08 | 2015-11-04 | 青岛青缆科技有限责任公司 | 新型阻燃xlpe绝缘电线电缆及其制备方法 |
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