CN111363605B - 一种防覆冰润滑脂及其制备方法和应用 - Google Patents
一种防覆冰润滑脂及其制备方法和应用 Download PDFInfo
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Abstract
一种防覆冰润滑脂及其制备方法和应用,将纳米硅溶胶、氨水、去离子水、正硅酸四乙酯、疏水处理剂分散于无水乙醇中,在水浴锅中连续搅拌,即可获得超疏水超亲油涂料;将超疏水超亲油涂料放置于烘箱中干燥,再将干燥后的块体进行研磨,获得超疏水超亲油纳米颗粒团聚物粉体;将超疏水超亲油纳米颗粒粉体、未改性润滑脂和硅油分散于有机稀释剂中,再在超声波清洗器中超声,获得均匀分散的混合乳液;将均匀分散的混合乳液置于烘箱中,获得半固态胶状物,再在室温下静置挥发残余的有机稀释剂,即可获得改性后的防覆冰润滑脂。本发明所述防覆冰润滑脂涂覆工艺对基底要求低,且对平面或曲面没有要求,可大面积配制施工,有利于防覆冰润滑脂的推广和应用。
Description
技术领域
本发明属于涂层的制备和应用技术领域,涉及一种防覆冰润滑脂及其制备方法和应用。
背景技术
长期以来,固体表面积冰给人们的日常生活带来了一系列严峻的问题,包括干扰飞机飞行、切断电源线、干扰风机叶片流场等。飞机在飞行过程中,厚度约为1.2毫米的冰粘附在机翼表面,将导致单位面积升力降低25%;输电线绝缘层上冰的严重积聚会消除其电气绝缘,从而可能威胁输电系统或电信系统的安全;风机在恶劣环境下的叶片覆冰会严重影响电力系统的正常运行,造成发电量的损失,减少机组设计寿命。积冰带来的麻烦还远不止这些,因此,有效地开展防冰研究具有重大的意义和价值。
目前已发展的防冰/除冰技术皆有自身弊端。传统的被动除冰技术有加热除冰、液体除冰和机械除冰等。加热除冰需表面结冰达到一定程度,能量消耗大;液体除冰系统复杂,且在飞行器飞行时无效;机械除冰存在除冰周期长、对材料表面破坏严重、成本高等问题,与此同时冰层的脱落十分困难。新兴的主动防冰技术主要有两种,一是利用超疏水涂层的超疏水性来延迟结冰;二是利用界面润滑涂层将固-固界面转变为固-液-固界面,从而极大地降低冰粘附力。但是超疏水涂层在粗糙度增大的情况下,一旦结冰,冰粘附强度迅速增大;界面润滑涂层易污染且无法实现自清洁,实际应用起来比较困难;与此同时,二者在-80℃及以下的超低温环境下积冰大量存在且难以去除。
基于此,本发明利用硅溶胶和低表面能物质配制得到乙醇基超疏水超亲油涂料,高温蒸发及室温干燥后通过研磨筛粉得到具有一定粒径大小的超疏水超亲油纳米颗粒粉体。将一定比例的润滑脂、超疏水超亲油纳米颗粒粉体和硅油在有机稀释剂中混合,利用超声和磁力搅拌得到均匀分散的混合乳液,之后将乳液放置在特定温度下烘干,进而获得改性后的防覆冰润滑脂。防覆冰润滑脂可满足-150℃及以下环境温度下材料表面积冰在较小力作用去除的要求。
发明内容
解决的技术问题:本发明的目的是为了拓展润滑脂的应用范围,提供一种防覆冰润滑脂及其制备方法和应用。本发明采用的设备工艺简单、易操作,适合大规模制备生产。
技术方案:一种防覆冰润滑脂的制备方法,按比例计算,体积份单位为毫升,质量份单位为克,具体步骤包括:(1)超疏水超亲油涂料配制:将1-3质量份纳米硅溶胶、2-10体积份氨水、6-16体积份去离子水、0.1-1体积份正硅酸四乙酯、0.1-2体积份疏水处理剂分散于60-160体积份无水乙醇中,在40-80℃的水浴锅中连续搅拌12-48h,即可获得超疏水超亲油涂料;(2)超疏水超亲油纳米颗粒团聚物粉体制备:将超疏水超亲油涂料放置于80-150℃烘箱中12-24h进行干燥,再将干燥后的块体进行研磨,并用600目筛网筛分,获得超疏水超亲油纳米颗粒团聚物粉体,粒径大小为15-75μm;(3)混合乳液配制:将0.05-0.5质量份超疏水超亲油纳米颗粒粉体、1-10质量份未改性润滑脂和0.5-2.5质量份硅油分散于20-200质量份有机稀释剂中,搅拌10-30min,再在超声波清洗器中超声10-30min,再搅拌12-24h,获得均匀分散的混合乳液; (4)防覆冰润滑脂制备:将均匀分散的混合乳液置于80-120℃的烘箱中6-12h,获得半固态胶状物,再在室温下静置6-12h挥发残余的有机稀释剂,即可获得改性后的防覆冰润滑脂。
优选的,上述纳米硅溶胶中纳米颗粒尺寸为40-120nm,固含量10-20%,pH值4-5。
上述疏水处理剂是短链饱和脂肪酸、短链烷烃三甲氧基或三乙氧基硅烷中的至少一种。
上述有机稀释剂为无水乙醇、异丙醇、乙酸丁酯、醋酸乙酯中的一种。
上述未改性润滑脂具有如下特性:由65-95质量份基础油、5-25质量份钠盐、0-10质量份混合添加剂共混制得,滴点不小于250℃,在120℃下1h蒸发度小于2%;所述基础油为硅油、合成油、双酯油中的至少一种,所述钠盐为复合酰胺钠盐、脂肪酸酰胺钠盐、烷基对苯二甲酸酰胺钠盐中至少一种,所述混合添加剂中按质量比:磷酸三钠抗氧剂占30%,乙二胺四乙酸四苄基酰胺抗氧剂占20%,结构改善剂占30%,极压抗磨剂占20%。
上述结构改善剂为环烷酸皂、乙酸钙、油酸中的一种,极压抗磨剂为三氟氯乙烯调聚物、三甲苯磷酸酯、二硫代氨基甲酸氧化钼中的一种。
上述制备方法制得的防覆冰润滑脂。
上述防覆冰润滑脂在低温或超低温部件防覆冰中的应用。
应用具体步骤为:使用环境为-20℃低温环境下,使用线棒滚涂工艺在工件表面均匀涂敷一薄层,厚度在3μm-100μm;使用环境为-150℃及以下,使用刷涂工艺在工件表面均匀涂敷一层,厚度不小于0.5mm。
有益效果:(1)防覆冰润滑脂较其他润滑脂具有一定的疏水性,其水滴静态接触角大于120°,这使得疏水润滑脂具有优异的防污、防水性能。(2)超疏水超亲油纳米颗粒团聚物粉体和润滑脂纤维组织框架形成微纳复合结构,提高了润滑脂基础油的自锁能力,进而提高了润滑脂的流变性和润滑性。(3)本发明所述防覆冰润滑脂涂覆于工件表面,3μm厚涂层在-20℃低温环境下可延迟结冰30-180min,冰粘附强度5-10KPa,比未改性润滑脂的冰粘附强度降低了50-70%;0.5mm厚涂层在-150℃及以下超低温环境下可延迟结冰600-2000s,冰粘附强度为10-20KPa,比未改性润滑脂的冰粘附强度降低了65-85%。(4)本发明所述防覆冰润滑脂具有优异的宽温度使用范围,最高使用温度可达150℃,最低可在使用液氢液氧等低温气体的部件表面使用;防覆冰润滑脂具有良好的阻燃性,其滴点大于250℃。(5)本发明所述防覆冰润滑脂具有优异的可恢复能力,且不与液氧、液氢、液氮相溶。(6)制备防覆冰润滑脂所用有机稀释剂在配置混合乳液后沉降速度慢,且在室温下挥发速度较快,易于在加热情况下快速完成去除。(7)本发明所述防覆冰润滑脂制备设备要求低,具备超声分散和机械搅拌的器材即可;制备原材料易得,如所述有机溶剂为酒精,所述疏水处理剂为低表面能物质;制备方法易操作,将超疏水超亲油纳米颗粒团聚物粉体与润滑脂在有机稀释剂中均匀混合后烘干即可获得。(8)本发明所述防覆冰润滑脂涂覆工艺对基底要求低,金属、无机材料、聚合物等硬质或软质表面均可进行涂覆,且对平面或曲面没有要求,可大面积配制施工,有利于防覆冰润滑脂的推广和应用。
附图说明
图1. 实施例1中润滑脂涂敷在铝合金片上的光学图及其水滴静态接触角光学图和油滴静态接触角光学图; 其中a展示的是水滴静态接触角,b展示的是油滴静态接触角;
图2. 实施例2中改性前后润滑脂的扫描电子图片;a为传统润滑脂的SEM图, b为防覆冰润滑脂的SEM图;
图3. 实施例3中润滑脂进行-20℃低温及-150℃超低温下冰粘附强度的测试结果图;a为-20℃低温环境,b为-150℃超低温环境;
图4. 实施例4中润滑脂最高使用温度的表征。
图5. 实施例5中润滑脂不与液氮相溶的测试结果图。
图6. 实施例6中润滑脂面漆喷涂在铝合金片上的光学图及其水滴静态接触角光学图。
具体实施方式
实施例1
未改性润滑脂制备:(1)将25g脂肪酸酰胺钠盐分散于65g硅油中,在70℃的水浴锅中连续搅拌2h得到混合乳液;(2)将3g磷酸三钠抗氧剂、2g乙二胺四乙酸四苄基酰胺抗氧剂、3g环烷酸皂和2g三氟氯乙烯调聚物加入到混合乳液中,水浴锅升温至110℃保温6h后获取未改性润滑脂。
防覆冰润滑脂制备:(1)将1g纳米颗粒尺寸为40-100nm,固含量15%,pH值4的ST-OUP硅溶胶、4mL分析纯,含量38wt.%氨水、8mL去离子水、0.6mL TEOS、0.6mL三乙氧基辛基硅烷分散于80mL无水乙醇中,在50℃的水浴锅中连续搅拌24h得到超疏水超亲油涂料;(2)将超疏水超亲油涂料放置于120℃的烘箱中12h进行干燥,再将干燥后的块体进行研磨,并用300目筛网筛分后获得粒径大小为15-50μm的超疏水超亲油纳米颗粒团聚物粉体;(3)将0.08g超疏水超亲油纳米颗粒团聚物粉体、4g未改性润滑脂和0.8g硅油分散于50g乙酸丁酯中,先磁力搅拌20min,再超声10min,之后继续磁力搅拌24h后得到混合乳液;(4)将混合乳液置于80℃的烘箱中8h,获得半固态胶状物,再在室温下静置6h后获取改性后的防覆冰润滑脂。
经过该方法制备的润滑脂具有一定的疏水性和亲油性。其水滴静态接触角为124.3°,如图1(a);油滴静态接触角为12.4°,如图1(b)。
实施例2
将实施例1中制备的防覆冰润滑脂和传统润滑脂进行除油操作来对比观察二者微观组织结构上的异同。除油操作如下:将润滑脂样品均匀涂抹在薄铝片上,厚度为3μm,然后将涂有样品的铝片放入盛有石油醚的烧杯中,封口静置一段时间,待润滑脂中的基础油溶解于石油醚后将铝片取出。将样品进行喷金处理操作之后在场发射扫描电子显微镜下进行观察,结果如图2所示。其中,图2(a)为传统润滑脂的SEM图,图2(b)为防覆冰润滑脂的SEM图。对比可以看出,防覆冰润滑脂纤维框架被包覆了大量的超疏水超亲油纳米颗粒团聚物粉体,形成了微纳复合的组织结构,该结构可大大提高润滑脂基础油的自锁能力,抑制其挥发。
实施例3
对实施例1中制备的防覆冰润滑脂进行低温及超低温环境下除冰时冰粘附强度的测试:
(1) -20℃低温环境:使用线棒滚涂工艺在铝合金表面均匀涂敷一薄层防覆冰润滑脂,厚度为3μm;测试过程如图3(a)所示。
(2)-150℃超低温环境:使用刷涂工艺在铝合金表面均匀涂敷一层防覆冰润滑脂,厚度为0.5mm;测试过程如图3(b)所示。
测试结果为多次测试后求取平均值。在-20℃低温环境下,未改性润滑脂除冰时冰粘附强度为21.7KPa,防覆冰润滑脂为7.6KPa,除冰性能提高65.0%;在-150℃超低温环境下,未改性润滑脂除冰时冰粘附强度为65.2KPa,防覆冰润滑脂为16.6KPa,除冰性能提高74.5%。
实施例4
对实施例1中制备的防覆冰润滑脂进行最高使用温度的耐久性测试。在测试中加入混超双疏纳米颗粒团聚物粉体润滑脂进行对比分析。超双疏型润滑脂的制备工艺只需把防覆冰润滑脂制备流程步骤1中的三乙氧基辛基硅烷换成氟硅烷,其它步骤不变。将均匀涂敷润滑脂的铝合金样品分别放置在150℃烘箱中一定时间(0h,3h,6h, 12h,18h,24h,30h,36h,42h,48h),之后对高温处理过的铝合金样品进行-150℃下的冰粘附强度测试,测试结果如图4所示。
因为超双疏纳米颗粒团聚物粉体具有疏油性,超双疏型润滑脂在150℃条件下放置6h后,硅油挥发明显,从而导致润滑脂在-150℃下除冰时冰粘附强度大于30KPa。相反地,防覆冰润滑脂对内部基础油具有优异的自锁能力,所以在150℃条件下放置长达42h之后依旧满足超低冰粘附强度的要求。该测试表明疏水亲油型润滑脂具有优异的宽温度使用范围。
实施例5
对实施例1中制备的防覆冰润滑脂进行凝固再恢复和液氮不相溶测试。将防覆冰润滑脂均匀涂抹在薄铝片上,厚度为0.5mm,之后将其放置在装有液氮的不锈钢杯中30min。测试过程中的状态图如图5所示。结果表明,防覆冰润滑脂不与液氮相溶。将润滑脂在液氮中取出后,凝固的润滑脂再次恢复成半固态,说明防覆冰润滑脂具有优异的可恢复能力。
实施例6
(1)将1g纳米颗粒尺寸为40-100nm,固含量15%,pH值4的ST-OUP硅溶胶、4mL分析纯,含量38wt.%的氨水、8mL去离子水、0.6mL TEOS、0.3mL三乙氧基辛基硅烷分散于80mL无水乙醇中,在50℃的水浴锅中连续机械搅拌24h得到超疏水超亲油涂料;(2)将超疏水超亲油涂料放置于120℃的烘箱中12h进行干燥,再将干燥后的块体进行研磨,并用300目筛网筛分后获得粒径大小为15-50μm的超疏水超亲油纳米颗粒团聚物粉体;(3)将0.08g超疏水超亲油纳米颗粒团聚物粉体、4g未改性润滑脂和0.8g硅油分散于50g无水乙醇中,先磁力搅拌20min,再超声10min,之后在50℃水浴锅中磁力搅拌24h后得到防覆冰润滑脂涂料。
经过该方法获得的防覆冰润滑脂涂料具有优异的疏水性。如图6所示,其水滴静态接触角为142.7°;在-20℃环境下,未喷涂防覆冰润滑脂涂料的铝合金表面除冰时的冰粘附强度测试结果为168.0KPa,喷涂防覆冰润滑脂涂料的铝合金表面除冰时的冰粘附强度测试结果为12.8KPa,除冰性能提高92.4%。
Claims (8)
1.一种防覆冰润滑脂的制备方法,其特征在于按比例计算,体积份单位为毫升,质量份单位为克,具体步骤包括:(1)超疏水超亲油涂料配制:将1-3质量份纳米硅溶胶、2-10体积份氨水、6-16体积份去离子水、0.1-1体积份正硅酸四乙酯、0.1-2体积份疏水处理剂分散于60-160体积份无水乙醇中,在40-80℃的水浴锅中连续搅拌12-48h,即可获得超疏水超亲油涂料;(2)超疏水超亲油纳米颗粒团聚物粉体制备:将超疏水超亲油涂料放置于80-150℃烘箱中12-24h进行干燥,再将干燥后的块体进行研磨,并用600目筛网筛分,获得超疏水超亲油纳米颗粒团聚物粉体,粒径大小为15-75μm;(3)混合乳液配制:将0.05-0.5质量份超疏水超亲油纳米颗粒粉体、1-10质量份未改性润滑脂和0.5-2.5质量份硅油分散于20-200质量份有机稀释剂中,搅拌10-30min,再在超声波清洗器中超声10-30min,再搅拌12-24h,获得均匀分散的混合乳液,所述未改性润滑脂具有如下特性:由65-95质量份基础油、5-25质量份钠盐、0-10质量份混合添加剂共混制得,滴点不小于250℃,在120℃下1h蒸发度小于2%;所述基础油为硅油、合成油、双酯油中的至少一种,所述钠盐为复合酰胺钠盐、脂肪酸酰胺钠盐、烷基对苯二甲酸酰胺钠盐中至少一种,所述混合添加剂中按质量比:磷酸三钠抗氧剂占30%,乙二胺四乙酸四苄基酰胺抗氧剂占20%,结构改善剂占30%,极压抗磨剂占20%; (4)防覆冰润滑脂制备:将均匀分散的混合乳液置于80-120℃的烘箱中6-12h,获得半固态胶状物,再在室温下静置6-12h挥发残余的有机稀释剂,即可获得改性后的防覆冰润滑脂。
2.根据权利要求1所述防覆冰润滑脂的制备方法,其特征在于所述纳米硅溶胶中纳米颗粒尺寸为40-120nm,固含量10-20%,pH值4-5。
3.根据权利要求1所述防覆冰润滑脂的制备方法,其特征在于所述疏水处理剂是短链饱和脂肪酸、短链烷烃三甲氧基或三乙氧基硅烷中的至少一种。
4.根据权利要求1所述防覆冰润滑脂的制备方法,其特征在于所述有机稀释剂为无水乙醇、异丙醇、乙酸丁酯、醋酸乙酯中的一种。
5.根据权利要求1所述防覆冰润滑脂的制备方法,其特征在于所述结构改善剂为环烷酸皂、乙酸钙、油酸中的一种,极压抗磨剂为三氟氯乙烯调聚物、三甲苯磷酸酯、二硫代氨基甲酸氧化钼中的一种。
6.权利要求1-5任一所述制备方法制得的防覆冰润滑脂。
7.权利要求6所述防覆冰润滑脂在低温或超低温部件防覆冰中的应用。
8.根据权利要求7所述的应用,其特征在于:使用环境为-20℃低温环境下,使用线棒滚涂工艺在工件表面均匀涂敷一薄层,厚度在3μm-100μm;使用环境为-150℃及以下,使用刷涂工艺在工件表面均匀涂敷一层,厚度不小于0.5mm。
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