CN116640509B - 一种耐高温有机硅涂料 - Google Patents
一种耐高温有机硅涂料 Download PDFInfo
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Abstract
本发明公开了一种耐高温有机硅涂料,其包括有机硅树脂、低熔点玻璃粉、纳米添加剂、填料及助剂,通过将有机硅树脂、低熔点玻璃粉、纳米添加剂、填料及助剂进行混合,将混合物放入研磨分散多用机的研钵中研磨,经研磨后,过滤混合物,获得混合均匀的产品。本发明中,二硫化钼和低熔点玻璃粉对涂层的耐高温性能影响较大,二硫化钼和改性低熔点玻璃粉协同有机硅树脂,可提高涂料的耐高温性能及防腐性能。
Description
技术领域
本发明涉及耐高温有机硅涂料技术领域,具体涉及一种耐高温有机硅涂料。
背景技术
在钢结构和大型机械设备以及各种高炉、壁炉、锅炉、热风炉、排气管、换热器、油气田管道等都有需要采用耐高温涂层防护。
大多数有机涂料在200℃以上就会受热断键分解或产生其他副反应,耐高温涂层通常是指在200℃以上的温度下不会变色或剥离漆膜,仍能保持适当的物理机械性能的涂料,是使被保护对象在高温环境中仍能正常发挥作用的特种功能性涂料。
环氧树脂是具有附着力强,力学性能高,耐酸耐碱性强、漆膜坚韧,耐磨等的优点,应用广泛,但是其在高温下发生分子链断裂、重新交联,会造成涂层失效,无法满足高温环境下防腐需求,耐候性差,在长久的日照环境下,漆膜易发生粉化,韧性差,容易发生胺白现象。涂料聚氨酯树脂具有良好的耐水性、耐磨性、耐久性、柔软性,还有高硬度等优点,可以低温固化,缺点是价格昂贵、有使用期限、做底漆需要喷砂处理的底材。
发明内容
本发明的目的就是通过配方设计提高基础树脂的耐高温性能,以增加在翅片型铝材换热器的使用寿命,从而达到耐高温防腐的目的。
为实现上述目的,本发明的技术方案是提供了
一种耐高温有机硅涂料,其包括有机硅树脂、低熔点玻璃粉、纳米添加剂、填料及助剂,通过将有机硅树脂、纳米添加剂、填料及助剂进行混合,将混合物放入研磨分散多用机的研钵中研磨,经过4至5小时的研磨后,过滤混合物,获得混合均匀的产品。
进一步的,其还包括二甲苯,通过在上述研磨后的混合物中加入二甲苯来调节涂料的粘度。
进一步的,所述有机硅树脂选用瓦克Ren60。
进一步的,所述填料包括钛白粉或高钛粉、绢云母粉、硅灰石矿纤及气相二氧化硅中的至少一种及以上。
进一步的,所述助剂选用附着力促进剂MP-200或SiC-6655Fl中的一种或两种。
进一步的,所述纳米添加剂为二硫化钼。
进一步的,按重量份,所述涂料包括有机硅树脂30-60份、低熔点玻璃粉1-5份、二硫化钼1-5份、高钛粉2-10份、绢云母粉5-15份、硅灰石矿纤2-4份、气相二氧化硅0-0.75份、SiC-6655Fl附着力促进剂0-1份、二甲苯3-10份。
进一步的,所述二硫化钼制备方法如下:把四水钼酸铵与硫脲溶解在去离子水中,搅拌混合,而后将混合后的溶液转移到高压反应釜中,在150-250℃下加热15-25小时,然后冷却至室温,得到黑色产物;之后离心洗涤、干燥,得到干燥黑色二硫化钼粉末。
进一步的,所述低熔点玻璃粉为经改性处理的低熔点玻璃粉,所述改性低熔点玻璃粉的制备步骤如下:
(1)将低熔点玻璃粉与分散剂混合并加入到水中,而后在水浴中加热搅拌;
(2)在步骤(1)中再加入硬脂酸和偶联剂,并用玻璃棒适当搅拌,保证混合物均匀;
(3)将烧杯放置在磁力搅拌器中水浴加热搅拌,并保持温度恒定在80-120℃,持续时间为1-3h;最后,将充分混合的溶液经过抽滤和干燥,得到改性后的低熔点玻璃粉。
进一步的,所述分散剂采用六偏磷酸钠、三乙基己基磷酸、脂肪酸聚乙二醇酯或聚丙烯酸酯类中的一种或多种。
进一步的,所述低熔点玻璃粉为经改性处理的低熔点玻璃粉,所述改性低熔点玻璃粉的制备步骤如下:
(1)按重量份,将20-30份低熔点玻璃粉与2-5份六偏磷酸钠混合并加入到80-100份水中,而后在70-90℃水浴中加热搅拌12-18h;
(2)在步骤(1)中再加入1-5份硬脂酸和2-8份偶联剂,并用玻璃棒适当搅拌30分钟,保证混合物均匀;
(3)将烧杯放置在磁力搅拌器中水浴加热搅拌,并保持温度恒定在100℃,持续时间为1.5h;最后,将充分混合的溶液经过抽滤和干燥,得到改性后的低熔点玻璃粉。
进一步的,所述偶联剂为硅烷偶联剂,选自KH550、KH560、KH570、KH792、DL602、DL171中的一种;优选硅烷偶联剂KH570。
本发明的优点和有益效果在于:
本发明中,二硫化钼和低熔点玻璃粉对涂层的耐高温性能影响较大,二硫化钼和改性低熔点玻璃粉协同有机硅树脂,可提高涂料的耐高温性能及防腐性能;气相二氧化硅、绢云母粉对涂层的耐高温性能起到补强的作用;硅灰石矿纤对涂层起到了增韧的作用;附着力促进剂的加入对涂料附着力和分散性都起到一定的改善作用。本发明在有机硅树脂、二硫化钼及改性低熔点玻璃粉的协同复配下,可有效提高涂料的耐高温性能及防腐性能。
具体实施方式
下面结合实施例,对本发明的具体实施方式作进一步描述。以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
有机硅树脂Ren60:固体质量分数60%/>德国瓦克公司;
绢云母粉,徐州万桥绢云母厂;
钛白粉R-95,上海凯茵化工有限公司;
硅灰石矿纤,江西奥特科技有限公司;
低熔点玻璃粉,灵寿县硕隆矿产;
高钛粉,湖南新威凌新材料有限公司;
气相二氧化硅H30RM,德国瓦克公司;
马弗炉,S-2.5-12,天津市中环试验电炉有限公司;
电热鼓风干燥箱DHG-9030B。
(一)涂料制备
实施例1-3各组分的重量份,如下表所示:
实施例1 | 实施例2 | 实施例3 | |
有机硅树脂 | 30 | 45 | 60 |
二硫化钼 | 5 | 8 | 1 |
低熔点玻璃粉 | 1 | 5 | 2.5 |
气相二氧化硅 | 0.75 | 0.2 | 0.5 |
高钛粉 | 10 | 8 | 2 |
绢云母粉 | 15 | 7.5 | 5 |
硅灰石矿纤 | 2.5 | 3 | 2 |
SiC-6655Fl | 1 | 1 | 0.5 |
二甲苯 | 3 | 8.5 | 10 |
对比例1-6各组分的重量份,如下表所示:
其中,实施例1-3及对比例1-4中,有机硅树脂采用瓦克Ren60;对比例5中,有机硅树脂采用陶氏道康宁RSN-0805。实施例1-3及对比例1-5中,低熔点玻璃粉均为改性低熔点玻璃粉,对比例6采用的未改性低熔点玻璃粉。
实施例1-3及对比例1-6的制备工艺如下:
将有机硅树脂、低熔点玻璃粉、二硫化钼、高钛粉、绢云母粉、硅灰石矿纤、气相二氧化硅、SiC-6655Fl附着力促进剂进行混合,将混合物放入研磨分散多用机的研钵中研磨,经过5小时的研磨后,过滤混合物,获得混合均匀的产品。
其中,二硫化钼粉末制备:使用水热法合成二硫化钼粉末。把1mmol四水钼酸铵(NH4)6Mo7O24·4H2O与30mmol硫脲(SC(NH2)2)溶解在35mL去离子水中,搅拌30分钟得到混合溶液,把溶液转移到50ml特氟龙内衬的高压反应釜中。在200℃下加热18小时,然后冷却至室温,得到黑色产物。使用去离子水和无水乙醇对黑色产物进行多次离心洗涤,然后在60℃干燥12小时,得到干燥黑色二硫化钼粉末。
实施例1-3及对比例1-5中,所述低熔点玻璃粉为经改性处理的低熔点玻璃粉,所述改性低熔点玻璃粉的制备步骤如下:
(1)按重量份,将25份低熔点玻璃粉与3份六偏磷酸钠混合并加入到80份水中,而后在90℃水浴中加热搅拌15h;
(2)在步骤(1)中再加入3份硬脂酸和5份硅烷偶联剂KH570,并用玻璃棒适当搅拌30分钟,保证混合物均匀;
(3)将烧杯放置在磁力搅拌器中水浴加热搅拌,并保持温度恒定在100℃,持续时间为1.5h;最后,将充分混合的溶液经过抽滤、60℃干燥5h,得到改性后的低熔点玻璃粉。
(二)涂层的制备
将实施例及对比例制备的涂料经下述方法制备涂层,其具体制备方法如下:
涂层的制备包括金属预处理、涂层的滴涂和高温烘烤固化。
金属预处理:指将铝材浸泡在强碱性溶液中(1mol/L的NaOH溶液),以产生浸蚀反应。该过程的目的是彻底去除表面污垢并清除铝表面的天然氧化膜,从而呈现出纯净的金属基体。为随后阳极氧化均匀导电、生成均匀阳极氧化膜打下良好的基础表面。
涂装方式:采取直接滴涂的方式将涂料淋到铝片表面。等待其表面干燥。
高温处理:将滴涂耐高温涂料的铝片置于马弗炉中,高温烘烤固化200℃1h。
(三)性能测试
将上述制备得到的涂层进行性能测试,具体如下:
耐高温性能测试:把试样置于马弗炉中,以50℃/min升至300-1100℃保温2h,放置冷却,待降至室温(25℃)后观察涂层是否产生开层、起皮、鼓泡、裂开等现象,记录涂层不开裂不起泡的温度。
耐腐蚀性:
耐酸测试:将涂有被测试涂料的试片放入25℃50%HCl溶液中;
耐碱测试:将涂有被测试涂料的试片放入25℃80%NaOH溶液中;每隔60min后观察涂层表面的情况,看涂层是否出现腐蚀,起泡,龟裂等异常情况来评估涂料的耐腐蚀性能。
实施例1-实施例3、对比例1-6所对应的的样板涂层检测结果如下表所示:
结合实施例2与对比例1-3可知,当涂料成分中未添加二硫化钼(对比例1)、未添加改性低熔点玻璃粉(对比例2)时,其耐热性能及耐腐蚀性能均较未添加气相二氧化硅(对比例3)的低,而对比例4中,二硫化钼和改性低熔点玻璃粉均未添加时,其耐高温性能及耐腐蚀性能最差,可见同时添加有二硫化钼、改性低熔点玻璃粉、气相二氧化硅的涂料,其耐高温性能及耐腐蚀性能最佳。此外,通过实施例2与对比例6可知,采用改性后的低熔点玻璃粉,其耐高温性能及耐腐蚀性能得到很大提高。
本发明中,二硫化钼和低熔点玻璃粉对涂层的耐高温性能影响较大,二硫化钼和改性低熔点玻璃粉协同有机硅树脂,可提高涂料的耐高温性能及防腐性能;气相二氧化硅、绢云母粉对涂层的耐高温性能起到补强的作用;硅灰石矿纤对涂层起到了增韧的作用;附着力促进剂的加入对涂料附着力和分散性都起到一定的改善作用。本发明在有机硅树脂、二硫化钼及改性低熔点玻璃粉的协同复配下,可有效提高涂料的耐高温性能及防腐性能。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (1)
1.一种耐高温有机硅涂料,其特征在于,按重量份,所述涂料由有机硅树脂30-60份、改性低熔点玻璃粉1-5份、二硫化钼1-8份、高钛粉2-10份、绢云母粉5-15份、硅灰石矿纤2-4份、气相二氧化硅0-0.75份、SiC-6655Fl附着力促进剂0-1份及二甲苯3-10份组成,
所述有机硅树脂选用瓦克Ren60;
所述改性低熔点玻璃粉的制备步骤如下:
(1)按重量份,将25份低熔点玻璃粉与3份六偏磷酸钠混合并加入到80份水中,而后在90℃水浴中加热搅拌15h;
(2)在步骤(1)中再加入3份硬脂酸和5份硅烷偶联剂KH570,并用玻璃棒适当搅拌30分钟,保证混合物均匀;
(3)将烧杯放置在磁力搅拌器中水浴加热搅拌,并保持温度恒定在100℃,持续时间为1.5h;最后,将充分混合的溶液经过抽滤和干燥,得到改性后的低熔点玻璃粉;
所述二硫化钼制备方法如下:把1mmol四水钼酸铵(NH4)6Mo7O24·4H2O与30mmol硫脲(SC(NH2)2)溶解在35mL去离子水中,搅拌30分钟得到混合溶液,把溶液转移到50ml特氟龙内衬的高压反应釜中;在200℃下加热18小时,然后冷却至室温,得到黑色产物;使用去离子水和无水乙醇对黑色产物进行多次离心洗涤,然后在60℃干燥12小时,得到干燥黑色二硫化钼粉末;
通过将瓦克Ren60、二硫化钼、改性低熔点玻璃粉、高钛粉、绢云母粉、硅灰石矿纤、气相二氧化硅、SiC-6655Fl附着力促进剂进行混合,将混合物放入研磨分散多用机的研钵中研磨,经研磨后,在研磨后的混合物中加入二甲苯,过滤混合物,获得混合均匀的产品。
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