CN104673009B - 一种水性隔音防腐涂料用乳液及其制备方法 - Google Patents
一种水性隔音防腐涂料用乳液及其制备方法 Download PDFInfo
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Abstract
本发明提供一种水性隔音防腐涂料用乳液及其制备方法。该水性隔音防腐涂料用乳液采用互穿网络聚合物(LIPN)乳液合成技术,体系包括网络Ⅰ和网络Ⅱ两部分,主要由原料苯乙烯、丙烯酸丁酯、二乙烯苯(DVB)、丙烯酸、N‑羟甲基丙烯酰胺、碱性pH值调节剂、乳化剂OP‑10和MS‑1、引发剂、缓冲剂和水制备得到。该隔音防腐乳液具有稳定性高、固体含量高、阻尼温域宽、阻尼损耗因数高、机械性能高等特点。
Description
技术领域
本发明涉及一种水性隔音防腐涂料用乳液及其制备方法,具体用于铁路轨道交通车体的具有高柔韧性、抗冲击性和耐候性、耐酸碱腐蚀、阻尼温域宽、阻尼抗振复合损耗因数高等特点的水性隔音阻尼涂料。本发明特别适用于车辆减振降噪领域。
背景技术
本发明涉及的水性隔音防腐涂料用乳液运用在车辆上。随着我国火车、地铁、高铁向高档化发展,对隔音防腐涂料的性能提出了更高的要求,要求在较宽温度范围内具有很好的隔音阻尼效果。目前国产涂料其低温阻尼性能不能满足铁标要求,主要是水性基体树脂材料性能达不到要求,存在水性隔音防腐乳液对底材的附着力及其持久性差、水性阻尼乳液温度大于或小于25℃阻尼性能降低、水性阻尼乳液固含量上不去从而影响施工性能等一系列不足。
互穿网络聚合物(IPN或LIPN)是一种独特的高分子共混物。它是由交联聚合物Ⅰ和交联聚合物Ⅱ各自交联后所得的网络连续地相互穿插而成的。IPN不同于接枝共聚物,因为在IPN中聚合物Ⅰ和Ⅱ之间未发生化学键结合;它也不同于相容的共混物,因为聚合物Ⅰ和Ⅱ在IPN中存在各自的相,虽然相分离的微区尺寸小到只有几百至一千埃。IPN的合成方法主要有分步法和同步法两种。分步法是将已经交联的聚合物(第一网络)置入含有催化剂、交联剂等的另一单体或预聚物中,使其溶胀,然后使第二单体或预聚体就地聚合并交联形成第二网络,所得产品称分步互穿聚合物网络。同步法,是将两种或多种单体在同一反应器中按各自聚合和交联历程进行反应,形成同步互穿网络。此外,由IPN的聚合机理决定了聚合物Ⅰ/聚合物ⅡIPN(聚合物Ⅰ为第一网络,聚合物Ⅱ为第二网络)的结构和性能不同于聚合物Ⅱ/聚合物ⅠIPN(聚合物Ⅱ为第一网络,聚合物Ⅰ为第二网络)。
虽然现有技术中已存在以互穿网络聚合物形成的涂料用乳液的报道,但本领域仍然需要研发一种具有阻尼温域宽、复合损耗因数高的水性隔音防腐涂料用乳液。
发明内容
为了解决现有技术中存在的上述技术问题,本发明的目的是提供一种水性隔音防腐涂料用乳液及其制备方法。本发明的水性隔音防腐涂料用乳液采用互穿网络聚合物乳液合成技术,体系包括网络Ⅰ和网络Ⅱ两部分。主要由苯乙烯、丙烯酸丁酯、二乙烯苯、丙烯酸、N-羟甲基丙烯酰胺、氨水、乳化剂、引发剂、缓冲剂和水制备得到。
因此,本发明提供一种水性隔音防腐涂料用乳液,所述乳液由网络Ⅰ和网络Ⅱ以互穿网络聚合物(LIPN)乳液合成技术制备得到,其中,网络Ⅰ的原料包括苯乙烯30~40份、丙烯酸丁酯5~8份、二乙烯苯(DVB)0.1~0.2份、丙烯酸0.3~1份、乳化剂OP-10(辛烷基苯酚聚氧乙烯醚)和MS-1(烷基酚醚磺基琥珀酸酯钠盐)、引发剂、碱性pH值调节剂、缓冲剂和水,网络Ⅱ的原料包括苯乙烯5~8份、丙烯酸丁酯50~55份、二乙烯苯(DVB)0.1~0.2份、N-羟甲基丙烯酰胺0.1~0.5份、引发剂、碱性pH值调节剂和水。
优选地,所述乳化剂OP-10为0.5~1.0份和MS-1为3.0~5.0份。本发明中通过使用特定成份和份量的(网络Ⅰ和网络Ⅱ)单体、特定成份和份量的复配乳化剂,使得本发明制备得到的水性隔音防腐涂料用乳液具有阻尼温域宽、复合损耗因子高的特点。用本乳液配制的阻尼涂料在-10~50℃连续温域内具有很好的阻尼效果,其复合损耗因数大于等于0.05且小于等于1.7。
优选地,所述网络Ⅰ和网络Ⅱ中的引发剂均为过硫酸钾和/或过硫酸铵,且网络Ⅰ和网络Ⅱ中的引发剂均为0.2~0.3份。
优选地,所述网络Ⅰ和网络Ⅱ中的碱性pH值调节剂均为氨水,其用量在网络Ⅰ和网络Ⅱ中均为0.1~0.5份。
优选地,所述缓冲剂选自磷酸氢钠、磷酸氢二钠和碳酸氢钠中的一种或多种,其用量为0.1~0.3份。
在一种具体的实施方式中,所述网络Ⅱ中还含有缓冲剂0.1~0.3份。
优选地,所述网络Ⅰ中的水为80~100份,网络Ⅱ中的水为10~20份。
在一种具体的实施方式中,所述网络Ⅱ中还含有丙烯酸0.3~1份。
在一种具体的实施方式中,网络Ⅰ:苯乙烯30~40份;丙烯酸丁酯5~8份;DVB0.1~0.2份;丙烯酸0.3~1份;OP-100.5~1.0份;MS-13.0~5.0份;过硫酸钾0.2~0.3份;磷酸氢钠0.2~0.3份;氨水0.1~0.5份;水80~100份。网络Ⅱ:苯乙烯5~8份;丙烯酸丁酯50~55份;DVB(二乙烯苯)0.1~0.2份;N-羟甲基丙烯酰胺0.1~0.5份;氨水0.1~0.5份;过硫酸钾0.2~0.3份;水10~20份。
本发明还提供一种上述乳液的制备方法,包括如下步骤:
1)配制下述几种液体:将引发剂用水溶解配成引发剂溶液;另将苯乙烯、丙烯酸丁酯、丙烯酸、OP-10、MS-1、二乙烯苯及水按网络Ⅰ的原料份数配比进行预乳化,得到待滴加的预乳化液;并向反应容器中加入水和缓冲剂,搅拌,升温至65~75℃,得到缓冲液;
2)向所述缓冲液中同时滴加所述预乳化液和引发剂溶液,进行聚合反应,反应温度控制在75~90℃,同时控制滴加速度使反应物料在1.5~2.5h内滴完,反应中和/或反应后加入碱性pH值调节剂,降温静置,制得含网络Ⅰ的种子乳液;
优选步骤2)中降温为降至室温,静置时间为12小时左右。
3)将苯乙烯、丙烯酸丁酯、二乙烯苯、N-羟甲基丙烯酰胺及可选择的丙烯酸按网络Ⅱ的原料份数配比进行预混合,得到混合液;将所述混合液加入所述含网络Ⅰ的种子乳液中,搅匀静置,再将网络Ⅱ中所需的引发剂溶液滴加在其中,以与步骤2)相同范围的温度和滴加时间进行聚合反应,之后保温反应;并在反应中和/或反应后加入碱性pH值调节剂;得到所述水性隔音防腐涂料用乳液。
本领域技术人员可以理解的,网络Ⅱ中的水份最好是加在引发剂中或碱性pH值调节剂中,而本步骤的所述混合液中最好是不加水。此外,步骤3)中搅匀静置的时间例如为1小时。
本发明提供的隔音防腐乳液具有稳定性高、固体含量高、阻尼温域宽、复合损耗因数高、机械性能高等特点。本发明提供的隔音防腐乳液的制备方法简单易控,所得产品效果好。
具体实施方式
以下结合具体的实施例说明本发明,本发明的范围并不限于实施例中的方案。在本发明中,如无特殊说明,其中的份均指重量份。
实施例1
本例中的水性隔音防腐涂料用乳液由下述配比的原料制备得到。网络Ⅰ:苯乙烯30份;丙烯酸丁酯5份;DVB0.1份;丙烯酸0.5份;OP-100.5份;MS-13.0份;过硫酸钾0.2份;磷酸氢钠0.2份;氨水0.1份;水80份。网络Ⅱ:苯乙烯8份;丙烯酸丁酯55份;DVB0.2份;N-羟甲基丙烯酰胺0.5份;丙烯酸0.3份;氨水0.5份;过硫酸钾0.3份;水20份。
该水性隔音防腐涂料用乳液的制备方法为:
(1)将过硫酸钾用水溶解好,配成5%的溶液;
(2)将苯乙烯、丙烯酸丁酯、丙烯酸、OP-10、MS-1、DVB及水按网络Ⅰ设计配方量进行预乳化,待滴加;
(3)向四口烧瓶加入打底水、磷酸氢钠适量,搅拌,升温至70℃;
(4)预乳化单体和适量过硫酸钾水溶液同时以滴加方式进入四口烧瓶进行聚合反应,反应温度控制在80~85℃,同时控制滴加速度,使反应物料在1~1.5h内滴完,并加入氨水适量,降温至室温,静置12小时;
(5)将上述聚合得到的乳液作为种子乳液,将苯乙烯、丙烯酸丁酯、DVB、N-羟甲基丙烯酰胺及丙烯酸按网络Ⅱ量配比好,加入种子乳液中搅匀静置1小时后,将适量过硫酸钾水溶液滴加入反应物料中,反应温度控制在80~85℃,同时控制滴加速度,使反应物料在1~1.5h内滴完,最后保温反应2h,并加入氨水适量,完成聚合反应;得到所述隔音防腐阻尼涂料用乳液。
该水性隔音防腐涂料用乳液的检测和应用:该乳液配制成涂料后,经中国科学院声学计量测试站检测在各温度点下的复合损耗因素值,得:-10℃,0.05;20℃,0.18;50℃,0.06。说明本发明的产品在-10~50℃连续温域内具有很好的阻尼效果,其完全满足铁标要求(高于相应温度点下铁标要求的复合损耗因素值)-10℃,0.05;20℃,0.11;50℃,0.05。
实施例2
本例中的水性隔音防腐涂料用乳液由下述配比的原料制备得到。网络Ⅰ:苯乙烯40份;丙烯酸丁酯8份;DVB0.2份;丙烯酸1份;OP-101.0份;MS-15.0份;过硫酸钾0.3份;磷酸氢钠0.3份;氨水0.5份;水100份。网络Ⅱ:苯乙烯5份;丙烯酸丁酯50份;DVB 0.1份;N-羟甲基丙烯酰胺0.1份;氨水0.1份;过硫酸钾0.2份;水10份。
该水性隔音防腐涂料用乳液的制备方法与实施例1中产品的制备方法相同。
该水性隔音防腐涂料用乳液的检测和应用:该乳液配制成涂料后,经中国科学院声学计量测试站检测在各温度点下的复合损耗因素值,得:-10℃,0.062;20℃,0.152;50℃,0.055。说明本发明的产品在-10~50℃连续温域内具有很好的阻尼效果,其完全满足铁标要求的-10℃,0.05;20℃,0.11;50℃,0.05。
对比例1
本例中的水性隔音防腐涂料用乳液由下述配比的原料制备得到。网络Ⅰ:苯乙烯27份;丙烯酸丁酯10份;DVB0.2份;丙烯酸1份;OP-101.0份;MS-15.0份;过硫酸钾0.3份;磷酸氢钠0.3份;氨水0.5份;水100份。网络Ⅱ:苯乙烯8份;丙烯酸丁酯55份;DVB 0.1份;N-羟甲基丙烯酰胺0.1份;氨水0.1份;过硫酸钾0.2份;水10份。
该水性隔音防腐涂料用乳液的制备方法与实施例1中产品的制备方法相同。
该水性隔音防腐涂料用乳液的检测和应用:该乳液配制成涂料后,经中国科学院声学计量测试站检测在各温度点下的复合损耗因素值,得:-10℃,0.073;20℃,0.12;50℃,0.033。说明对比例中的该产品在-10~50℃连续温域内的阻尼效果一般(其高温区域隔音效果较差),无法满足铁标要求的-10℃,0.05;20℃,0.11;50℃,0.05。
从上述实施例和对比例可以看出,对比例1中仅有网络Ⅰ中的两种原料(苯乙烯和丙烯酸丁酯)的用量不在本发明的范围中,所得乳液的高温区域隔音效果就已经比较差。本发明只是示例性地列举了众多的对比例方案中的一种,以此说明本发明方案中各组分及其含量的不可或缺性。
Claims (4)
1.一种水性隔音防腐涂料用乳液,其特征在于,所述乳液由网络Ⅰ和网络Ⅱ以互穿网络聚合物乳液合成技术制备得到,其中,
网络Ⅰ的原料包括苯乙烯30~40份、丙烯酸丁酯5~8份、二乙烯苯0.1~0.2份、丙烯酸0.3~1份、乳化剂OP-10为0.5~1.0份和MS-1为3.0~5.0份、引发剂过硫酸钾和/或过硫酸铵0.2~0.3份、碱性pH值调节剂氨水为0.1~0.5份、缓冲剂0.1~0.3份和水80~100份,所述缓冲剂选自磷酸氢钠、磷酸氢二钠和碳酸氢钠中的一种或多种;
网络Ⅱ的原料包括苯乙烯5~8份、丙烯酸丁酯50~55份、二乙烯苯0.1~0.2份、N-羟甲基丙烯酰胺0.1~0.5份、引发剂过硫酸钾和/或过硫酸铵0.2~0.3份、碱性pH值调节剂氨水为0.1~0.5份和水10~20份。
2.根据权利要求1所述的乳液,其特征在于,所述网络Ⅱ中还含有缓冲剂0.1~0.3份。
3.根据权利要求1所述的乳液,其特征在于,所述网络Ⅱ中还含有丙烯酸0.3~1份。
4.一种如权利要求1或3所述的乳液的制备方法,包括如下步骤:
1)配制下述几种液体:
将引发剂用水溶解配成引发剂溶液;
另将苯乙烯、丙烯酸丁酯、丙烯酸、OP-10、MS-1、二乙烯苯及水按网络Ⅰ的原料份数配比进行预乳化,得到待滴加的预乳化液;
并向反应容器中加入水和缓冲剂,搅拌,升温至65~75℃,得到缓冲液;
2)向所述缓冲液中同时滴加所述预乳化液和引发剂溶液,进行聚合反应,反应温度控制在75~90℃,同时控制滴加速度使反应物料在1.5~2.5h内滴完,反应中和/或反应后加入碱性pH值调节剂,降温静置,制得含网络Ⅰ的种子乳液;
3)将苯乙烯、丙烯酸丁酯、二乙烯苯、N-羟甲基丙烯酰胺及可选择的丙烯酸按网络Ⅱ的原料份数配比进行预混合,得到混合液;将所述混合液加入所述含网络Ⅰ的种子乳液中,搅匀静置,再将网络Ⅱ中所需的引发剂溶液滴加在其中,以与步骤2)相同范围的温度和滴加时间进行聚合反应,之后保温反应;并在反应中和/或反应后加入碱性pH值调节剂;得到所述水性隔音防腐涂料用乳液。
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