CN114409899A - 一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法 - Google Patents
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Abstract
本发明提出的是一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,在常温下向反应釜中投入N‑乙基吡咯烷酮、聚乙烯蜡和偏苯三酸酐,升温并加入融化好的MDI‑100,保温结束后取样测定粘度,待树脂合格后关闭加热,加入N‑乙基吡咯烷酮和二甲苯,搅拌后,得到自润滑聚酰胺酰亚胺绝缘树脂成品。本发明在聚酰胺酰亚胺漆包线中引入润滑性良好的聚乙烯蜡,从而降低漆包线的最大静摩擦系数,制成的漆包线润滑效果好,既具有耐高温性能,又有良好自润滑性能和柔顺性能;制备工艺简单,省去涂制润滑涂层,极大提高漆包线的生产效率、绕线性能和绕组性能,可广泛应用于电机、电器、变压器特别是磁环线圈作绕组线。
Description
技术领域
本发明涉及一种,特别是一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,属于漆包线漆制造技术领域。
背景技术
聚酰胺酰亚胺简称PAI,是酰亚胺环和酰胺键有规则交替排列的一类聚合物。聚酰胺酰亚胺的强度是当今世界上任何工业未增强塑料不可比拟的,其拉伸强度超过172MPa,在1.8MPa负荷下热变形温度为274℃。聚酰胺酰亚胺在制造后还可能进行固态聚合,通过后固化增加分子量提供更优良的性能,后固化在260℃下发生,固化所需的时间和温度主要取决于零件的厚度和形状。聚酰胺酰亚胺可在220℃下长期使用,300℃下不失重,450℃左右开始分解。其粘接性、柔韧性及耐碱性更佳,可与环氧树脂互混交联固化,耐磨性良好。
聚酰胺酰亚胺具有优良的机械性能,本色料拉伸强度为190Mpa,模制塑料主要用于齿轮、辊子、轴承和复印机分离爪等。若采用直链结构的多元醇与多元酸,合成得到的树脂具有线性结构,柔韧性非常好,主要用于涂料行业;聚酰胺酰亚胺具有良好的耐烧蚀性能和高温、高频下的电磁性,对金属和其它材料有很好的粘接性能,适用于漆包线漆、浸渍漆、薄膜、层压板材、涂层和粘合剂等。
目前电线的线圈绕线工艺广泛采用高速自动绕线机进行,由于绕线时漆包线会受到摩擦和冲击等作用,漆包线的绝缘层易受到机械损伤,造成绝缘性能下降。为了减小在高速绕线时的漆包线表面摩擦系数,通常在漆包线上涂液体石蜡或固体石蜡等润滑剂,但是这种方法绕制的线圈在浸漆处理时与浸渍漆的相溶性欠佳,容易产生粘合不良等问题。因此需要对作为漆包线漆的聚酰胺酰亚胺绝缘树脂进行一定的改进,以克服上述缺陷。
发明内容
本发明的目的在于解决现有聚酰胺酰亚胺漆包线漆在使用过程中存在的上述问题,提出一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法。
本发明的技术解决方案:一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,具体包括如下步骤:
1)在常温下向反应釜中投入N-乙基吡咯烷酮、聚乙烯蜡和偏苯三酸酐,升温至45-50℃;
2)加入融化好的MDI-100,使反应液自行升温;
3)待反应液不再升温后开始手动升温,以15℃/h的速率升温至85℃,并保温1h,期间反应液由黄棕色浑浊逐渐变为棕黄色澄清状;
4)保温结束后以15℃/h的速率继续升温至155℃,并保温1h;
5)每隔30min取样测定树脂粘度,若粘度上涨趋势不明显,则以5℃/h的速率升温至162-165℃;若粘度上涨趋势明显,则在155℃下继续保温,直至树脂粘度变化范围稳定在2500-2800mPa·s之间,测定标准为:树脂:N-乙基吡咯烷酮=2:1(质量比);
6)待树脂合格后关闭加热,加入N-乙基吡咯烷酮和二甲苯,搅拌2h后检测树脂固含和粘度,
树脂粘度测定过程具体如下:
1)取约2.5ml树脂样品置于锥板粘度计下平板的正中心;
2)缓慢压下锥板,将树脂样品温度平衡到25±0.2℃;
3)待温度达到要求后,选择锥板粘度计的档位,测定直接锥板粘度。
树脂固含测定过程具体如下:
1)选择3个相同直径的铝箔皿,并标识;
2)将天平调零去皮,分别称取铝箔皿的质量,记为m0;
3)用一次性滴管加入1g树脂样品于铝箔皿中,精确到0.0001g,记为m;
4)将样品摊薄置于180℃烘箱中烘干1h,取出烘干的铝箔皿称重,记为m1;
5)按以下公式计算树脂固含X:X=[(m1-m0)/m]×100%。
最终得到自润滑聚酰胺酰亚胺绝缘树脂成品,各原料的质量配比具体如下:N-乙基吡咯烷酮:58-63%、聚乙烯蜡:7%-10%、偏苯三酸酐:9%-12%、MDI-100:15%-20%、二甲苯:5%-10%。
与现有技术相比,本发明的优点在于:
1)在聚酰胺酰亚胺漆包线中引入润滑性良好的聚乙烯蜡,从而降低漆包线的最大静摩擦系数,因此制成的漆包线润滑效果好,最大静摩擦系数在0.060左右,既具有耐高温性能,又有良好自润滑性能和柔顺性能;
2)制备工艺简单,省去了涂制漆包线时的润滑涂层,极大地提高了漆包线的生产效率,提高了绕线性能和绕组性能;
3)采用该方法制备的自润滑聚酰胺酰亚胺漆包线漆可用于制造高性能自润滑复合漆包线,该漆包线可广泛应用于电机、电器、变压器特别是磁环线圈作绕组线。
具体实施方式
下面根据实施例进一步说明本发明的技术方案。在本说明书的描述中,实施例的内容意指结合其描述的具体技术特征包含于本发明的至少一个实施方式中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施方式或示例。而且,描述的具体技术特征可以在任何的一个或多个实施方式或示例中以合适的方式结合。
实验原料:N-乙基-2-吡咯烷酮(NEP)、偏苯三酸酐(TMA)、聚乙烯蜡、MDI-100、二甲苯。
1)室温下投入原料NEP、TMA和聚乙烯蜡并升温至50℃左右,此时物料呈乳白色浑浊液;
2)待釜温达到50℃时,加入MDI-100并使其自行升温,此时物料由乳白色浑浊液变成黄绿色浑浊液;
3)待釜温有下降趋势时,以15℃/h升温至85℃并保温1h,期间物料在70-75℃变成棕黄色澄清液,在77-82℃颜色开始变深并且液面有气泡产生;
4)保温结束后继续以15℃/h升温至155℃左右,以2℃/h缓慢升温至164℃,每隔30min测样直至粘度在2500-2800mpa.s,根据粘度变化情况适当延长保温时间,树脂粘度测定标准:树脂:NEP=2:1;;
5)待粘度合格后关闭加热,加入后续的NEP和二甲苯,搅拌3h后测定粘度和固含;其中树脂粘度测定标准:25℃直接锥板粘度;树脂固含测定标准:180温度1g1h;
6)后续根据实际产品需要调整固含和粘度;
7)将自润滑聚酰胺酰亚胺树脂和普通的聚酰胺酰亚胺树脂按1:10比例调制成成品漆并涂线测定各项性能,结果如下:
实验表明本发明制备的自润滑聚酰胺酰亚胺树脂可以显著改善动摩擦系数,耐击穿电压也有较大提高。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (5)
1.一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,其特征在于:该方法具体包括如下步骤:
1)在常温下向反应釜中投入N-乙基吡咯烷酮、聚乙烯蜡和偏苯三酸酐,升温至45-50℃;
2)加入融化好的MDI-100,使反应液自行升温;
3)待反应液不再升温后开始手动升温,以15℃/h的速率升温至85℃,并保温1h,期间反应液由黄棕色浑浊逐渐变为棕黄色澄清状;
4)保温结束后以15℃/h的速率继续升温至155℃,并保温1h;
5)每隔30min取样测定树脂粘度,若粘度上涨趋势不明显,则以5℃/h的速率升温至162-165℃;若粘度上涨趋势明显,则在155℃下继续保温,直至树脂粘度变化范围稳定在2500-2800mPa·s之间;
6)待树脂合格后关闭加热,加入N-乙基吡咯烷酮和二甲苯,搅拌2h后检测树脂固含和粘度,得到自润滑聚酰胺酰亚胺绝缘树脂成品。
2.根据权利要求1所述的一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,其特征在于:所述步骤5)中树脂粘度测定标准为:树脂:N-乙基吡咯烷酮=2:1(质量比)。
3.根据权利要求1所述的一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,其特征在于:所述步骤6)中树脂粘度测定过程具体如下:
1)取约2.5ml树脂样品置于锥板粘度计下平板的正中心;
2)缓慢压下锥板,将树脂样品温度平衡到25±0.2℃;
3)待温度达到要求后,选择锥板粘度计的档位,测定直接锥板粘度。
4.根据权利要求1所述的一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,其特征在于:所述步骤6)中树脂固含测定过程具体如下:
1)选择3个相同直径的铝箔皿,并标识;
2)将天平调零去皮,分别称取铝箔皿的质量,记为m0;
3)用一次性滴管加入1g树脂样品于铝箔皿中,精确到0.0001g,记为m;
4)将样品摊薄置于180℃烘箱中烘干1h,取出烘干的铝箔皿称重,记为m1;
5)按以下公式计算树脂固含X:X=[(m1-m0)/m]×100%。
5.根据权利要求1所述的一种新型的自润滑聚酰胺酰亚胺绝缘树脂的合成方法,其特征在于:所述步骤6)中自润滑聚酰胺酰亚胺绝缘树脂成品中各原料的质量配比具体如下:N-乙基吡咯烷酮:58-63%、聚乙烯蜡:7%-10%、偏苯三酸酐:9%-12%、MDI-100:15%-20%、二甲苯:5%-10%。
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JPH05320340A (ja) * | 1992-05-27 | 1993-12-03 | Fujikura Ltd | 潤滑性ポリアミドイミドおよびその製法ならびに自己潤滑性絶縁電線 |
CN104449341A (zh) * | 2013-09-16 | 2015-03-25 | 丹阳四达化工有限公司 | 一种自润滑聚酰胺酰亚胺漆包线漆及其制备方法 |
CN106752894A (zh) * | 2016-12-29 | 2017-05-31 | 天恒达电工科技股份有限公司 | 一种自润滑聚酰胺酰亚胺漆包线漆的制备方法 |
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JPH05320340A (ja) * | 1992-05-27 | 1993-12-03 | Fujikura Ltd | 潤滑性ポリアミドイミドおよびその製法ならびに自己潤滑性絶縁電線 |
CN104449341A (zh) * | 2013-09-16 | 2015-03-25 | 丹阳四达化工有限公司 | 一种自润滑聚酰胺酰亚胺漆包线漆及其制备方法 |
CN106752894A (zh) * | 2016-12-29 | 2017-05-31 | 天恒达电工科技股份有限公司 | 一种自润滑聚酰胺酰亚胺漆包线漆的制备方法 |
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CN116253860A (zh) * | 2023-03-21 | 2023-06-13 | 南通百川新材料有限公司 | 一种自润滑聚氨酯绝缘树脂的合成方法 |
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