CN114752011A - 一种红外反射乳液的制备方法 - Google Patents
一种红外反射乳液的制备方法 Download PDFInfo
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- CN114752011A CN114752011A CN202210439967.4A CN202210439967A CN114752011A CN 114752011 A CN114752011 A CN 114752011A CN 202210439967 A CN202210439967 A CN 202210439967A CN 114752011 A CN114752011 A CN 114752011A
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- emulsion
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Abstract
本发明涉及节能材料技术领域，具体涉及一种红外反射乳液的制备方法，所述方法先将符合要求的红外反射粒子进行表面修饰，使其表面获得反应活性，再通过热引发乳液聚合，使红外反射粒子参与聚合，负载于乳液胶粒，本发明的方法使得红外反射粒子与乳液胶粒键合，负载稳固、分散均匀，其工艺简单、体系稳定，适用于多种红外反射粒子及乳液体系，具有一定的扩展性，且涉及工艺均为水性体系，环境友好，具有较高的实用价值和良好的应用前景。
Description
技术领域
本发明涉及节能材料技术领域，具体涉及一种红外反射乳液的制备方法。
背景技术
建筑外围护结构对太阳光的充分反射，可以有效降低室内冷负荷功率，从而降低能耗。在太阳能谱中，近红外区能量占比约为 50 ％，若选择性的反射近红外区能量，则可以在避免“光污染”的同时，有效节能。目前，常见的红外反射材料包括有机颜料、金属单质、金属化合物、掺杂金属氧化物等，受到广泛关注的材料包括氧化铟锡（ITO）、氧化锡锑（ATO）、铝参杂氧化锌（AZO）、镓参杂氧化锌（GZO）、二氧化钛（TiO2）等。
对于这些红外反射粒子（Infrared Reflective Particle, IRP），粒径越小，其比表面积越大，相同的粒子负载量，反射能力就越强，IRP 用量更少，对体系的影响更小。然而，粒径越小，IRP 的表面能越高。自然条件下，纳米、亚微米尺寸的 IRP 会自发团聚以降低表面能，导致比表面积减少，其太阳反射比和半球发射率显著降低。
因此，IRP 与有机组分复配使用时，需要解决粒子团聚的问题，国内外学者开展了许多相关研究工作。目前主要采用的方法有共混法、接枝共聚等。其中共混法主要是直接或进行表面修饰后，直接通过剪切力使 IRP 分散并使用，如中国专利 CN 113292888 A 中使用分散剂配制成分散液后与其他组分混合使用制备外墙保温防水涂料。
目前各类文献报导的合成方法中，物理共混法尚无法解决粒子团聚的问题，同时，通过物理共混获得的产物，小分子物质在外环境的影响下（如冻融循环）会向聚合物膜内/外表面迁移，造成系统整体性能下降。此外，与通过共价键负载相比，在聚合物逐渐老化断键的过程中，共混的粒子更易脱离而导致系统性能严重下降，这些都是亟需解决的问题。
发明内容
针对现有技术的缺陷，本发明的目的是提供一种红外反射乳液的制备方法，先通过对 IRP 进行表面修饰，再通过乳液聚合，在聚合的同时完成粒子负载，有效提高了有机红外反射涂层在生产过程中的 IRP 的分散性与稳定性，大大增强了红外反射乳液耐久性。
本发明解决技术问题采用如下技术方案：
一种红外反射乳液的制备方法，所述方法包括：
对红外反射粒子进行表面修饰，使其表面获得反应活性；
将修饰后的红外反射粒子与单体乳液聚合，使其负载于乳液胶粒。
优选地，所述红外反射粒子粒径为亚微米级，所述红外反射粒子表面存在羟基。
优选地，所述红外反射粒子粒径不超过500纳米，所述红外反射粒子包括氧化锡锑、二氧化钛和二氧化硅中的一种或几种。
优选地，所述对红外反射粒子进行表面修饰具体包括：
将红外反射粒子加入到乙醇中进行脉冲超声分散，加入氨水调节 pH 至弱碱性，添加匹配官能团的偶联剂，加热到预设温度，保温至反应完成后润洗分离即可；
所述偶联剂包括钛酸酯偶联剂、硅烷偶联剂中的一种或几种。
优选地，所述单体包括丙烯酸酯类单体、苯乙烯单体、丙烯酸单体中的一种或几种，所述丙烯酸酯类单体包括丙烯酸正丁酯、丙烯酸乙酯中的一种或几种。
优选地，所述将修饰后的红外反射粒子与单体乳液聚合具体包括：
将单体、修饰后的红外反射粒子加入到含有乳化剂、引发剂的水溶液中，充分分散后，通入氮气除去氧气，在预定温度下反应，并通过搅拌提供剪切力，反应结束后加入聚乙二醇（PEG），并调节乳液体系 pH。
优选地，所述乳液体系中单体含量为2-60 wt％，乳液体系调节后的pH值大于7。
优选地，所述乳化剂为阴离子乳化剂和非离子乳化剂组成的复配乳化剂，且阴离子乳化剂和非离子乳化剂的质量比为 3:1-6。
优选地，所述阴离子乳化剂为十二烷基苯磺酸钠，所述非离子乳化剂为壬基酚聚氧乙烯醚，所述水溶液中的水为去离子水且电导率≤25μS/cm。
优选地，所述单体预先进行纯化去阻聚剂处理，所述引发剂预先进行纯化去除稳定剂处理；
所述充分分散为采用超声分散，并在分散时使用冰水浴控制超声温度不超过10℃。
与现有技术相比，本发明具有如下的有益效果：
本发明相对于共混法可以提升 IRP 的分散性、稳定性，通过共聚负载 IRP，可以在一定程度提升红外反射性能的耐久性，本发明将符合要求的红外反射粒子进行表面修饰，使其表面获得反应活性，再通过热引发乳液聚合，使红外反射粒子参与聚合，负载于乳液胶粒，通过红外反射粒子与乳液胶粒键合，使得负载稳固，分散均匀与已有工艺相比，本方法工艺简单，体系稳定，粒子分散性好，特别的本发明进行 IRP 表面修饰获得可进行后续乳液聚合反应的官能团，因此通过更换具有相应官能团的偶联剂，即可适用于不同单体的乳液聚合体系，具有一定的扩展性，此外，由于本发明对于单体的选择较为广泛，因此，合成的红外反射乳液具有一定的通用性，可直接涂刷于中空玻璃内表面，起到对红外光阻隔的效果。同时，该乳液还可用于配制多彩涂料、真石漆、外墙罩面涂料、装饰砂浆罩面层等外墙节能产品，具有很强的适用性。
附图说明
通过阅读参照以下附图对非限制性实施例所作的详细描述，本发明的其它特征、目的和优点将会变得更明显：
图1为实施例1中红外反射乳液的制备方法工艺流程及原理示意图；
图2为实施例1中使用溶胶-凝胶法合成的SiO2的SEM图；
图3为实施例1中经过表面修饰后的SiO2的SEM图。
具体实施方式
下面结合具体实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明提供了一种红外反射乳液的制备方法，该乳液通过热引发单体聚合的一步反应，将表面修饰的 IRP负载于聚合物主链。本领域技术人员可借鉴本发明，适当改进合成工艺以实现本发明内容，如替换具有其他表面羟基的 IRP、替换不同官能团的单体。需要指出的是，所有类似的替换和改动对本领域技术人员来说是显而易见的，它们仍属于本发明的保护范围。本发明的方法及应用已经通过实施例对本发明进行了详细地描述，相关人员明显能在不脱离本发明内容、精神和范围内，对本文的方法和实际应用进行改动、替换或组合，来实现和应用本发明技术。
实施例1.
如图1所示，本实施例的一种红外反射乳液的制备方法，所述方法包括：
对红外反射粒子进行表面修饰，使其表面获得反应活性，通过对 IRP 的表面修饰，使其具有反应活性，修饰后的 IRP 记做 m-IRP；其中红外反射粒子粒径为亚微米级，红外反射粒子表面存在羟基，红外反射粒子粒径不超过500纳米，所述红外反射粒子包括氧化锡锑、二氧化钛和二氧化硅中的一种或几种，对红外反射粒子进行表面修饰具体包括：
将红外反射粒子加入到乙醇中进行脉冲超声分散，加入氨水调节 pH 至弱碱性，添加匹配官能团的偶联剂，加热到预设温度，保温至反应完成后润洗分离即可；
所述偶联剂包括钛酸酯偶联剂、硅烷偶联剂中的一种或几种，例如根据后续乳液聚合单体的官能团，采用对应不同官能团的硅烷偶联剂，如，KH570，KH550。
本实施例中IRP 包括但不限于 ATO、TiO2、SiO2 等需要控制粒径为亚微米级，可通过例如但不限于研磨、溶胶-凝胶合成法等方法控制粒径（亚微米级或更低），例如ATO 等粒子可采用研磨法以纳米砂磨机等直接研磨到需要粒径，TiO2、SiO2 等可采用溶胶-凝胶法，以 Stober 法合成 SiO2 为例，一定量的乙醇、氨水、正硅酸四乙酯（TEOS）加入到烧杯中，在室温（25℃）下使用磁力搅拌一定时间（如 24 小时）。其中，通过氨水的添加比例可调节粒径；
将上述粒径符合要求的 IRP 加入一定量的乙醇中，进行脉冲超声分散，加入氨水调节 pH 至弱碱性，加入含有特定官能团硅烷偶联剂，加热到预设温度，并保持一段时间。反应完成后，润洗分离，获得表面修饰的 IRP（m-IRP）；
进一步举例说明以 SiO2 为例，将 100 mL 乙醇、8 mL 氨水、4 mL TEOS加入反应器中，封口后控制反应温度为 25 °C，磁力搅拌 24 小时，反应结束后，离心分离，转速4000 rpm，时间 5 min，取离心管底部沉淀物，加入乙醇超声，离心、超声重复 3 次后，将获得的样品置于鼓风干燥箱中，60 °C 干燥 24 h 后备用，获得的符合粒径要求的IRP，SEM图如图 2 所示，使用溶胶-凝胶法合成的 SiO2，平均粒径约：240 nm，多分散指数（PDI）：1.0074；
将上述制备的IRP加入乙醇中（固含量约 15 wt%），使用超声分散均匀，加入氨水调节分散液 pH 为 7.5-8，加入 2-5 mL 硅烷偶联剂 KH570，保持 70°C，采用机械搅拌，搅拌速度约为 90 rpm，冷凝回流 24 h，获得 IRP 分散液；
除去未反应的偶联剂与共沉淀物：取出分散液，使用离心机进行离心，转速4000rpm，时间 5 min，使用丙酮作为润洗液，超声功率，超声 5 min,重复以上步骤，共 3 次。取底部沉淀物，置于真空干燥箱中常温干燥至恒重（约 20 小时），获得具有双键表面改性的m-IRP，如图3所示，使用经过表面修饰后的 SiO2，平均粒径约：350 nm，多分散指数（PDI）：1.0023；
将修饰后的红外反射粒子与单体乳液聚合，使其负载于乳液胶粒，其中单体包括丙烯酸酯类单体、苯乙烯单体、丙烯酸单体中的一种或几种，所述丙烯酸酯类单体包括丙烯酸正丁酯、丙烯酸乙酯中的一种或几种，本实施例将修饰后的红外反射粒子与单体乳液聚合具体包括：
将单体、修饰后的红外反射粒子加入到含有乳化剂、引发剂的水溶液中，充分分散后，通入氮气除去氧气，在预定温度下反应，并通过搅拌提供剪切力，反应结束后加入聚乙二醇（PEG），并调节乳液体系 pH，例如以苯丙乳液为例，制备方法为：将 m-IRP、苯乙烯、丙烯酸酯类单体、丙烯酸加入含有 KPS、OP-10、 SDBS 、的水溶液中，充分分散后，通入氮气除去氧气，在预定温度（70°C）反应一定时间（如 24 小时），并通过搅拌保证足够的剪切力，聚合结束后，加入 PEG，并调节体系 pH，获得红外反射乳液。同时获得的负载有 IRP 的丙烯酸酯类乳液，根据单体的不同，可广泛用于建筑外围护结构（门窗、外墙、屋面等）的节能领域；
在本实施例中最终制备的乳液体系中单体含量为2-60 wt％，乳液体系调节后的pH值大于7，乳化剂为阴离子乳化剂和非离子乳化剂组成的复配乳化剂，且阴离子乳化剂和非离子乳化剂的质量比为 3:1-6，在本实施例中阴离子乳化剂为十二烷基苯磺酸钠，非离子乳化剂为壬基酚聚氧乙烯醚，水溶液中的水为去离子水且电导率≤25μS/cm，单体预先进行纯化去阻聚剂处理，所述引发剂预先进行纯化去除稳定剂处理；充分分散为采用超声分散，并在分散时使用冰水浴控制超声温度不超过10℃；
进一步举例说明：在反应器中加入单体、乳化剂、引发剂、m-IRP。单体选择丙烯酸酯类（如丙烯酸甲酯、丙烯酸正丁酯等）、丙烯酸、苯乙烯等，单体需先纯化去阻聚剂，精制后的单体用量为30 - 50 g，优选为 50 g，乳化剂包括阴离子乳化剂、非离子乳化剂，例如十二烷基苯磺酸钠、壬基酚聚氧乙烯基醚，用量共计：0.5-1.5 g，优选为 1 g，引发剂（使用前需纯化去除稳定剂），例如过硫酸钾，用量为 1-3 g，优选 1 g，m-IRP 0.5-2 g，优选 1 g，组分添加完成后，使用超声分散，功率为1000 W，时间为5 min，超声时需使用冰水浴控制超声温度，温度不超过 10 °C，通氮除氧，时间为10 min，完成后升温至 75 °C，引发聚合，冷凝回流，并使用机械搅拌，搅拌速度约为 90 rpm。反应时间为 8-24 h，反应完成后，滴加NaHCO3 溶液，将乳液 pH 值调节到 7-8，在这里乳液制备最后一步均需要添加聚乙二醇，此处聚乙二醇（PEG)是作为分散剂使用，通过 PEG 的空间位阻作用，防止胶粒为了降低表面张力而发生团聚，一般来说，最后添加的 PEG 的并不影响乳胶粒的化学性质，只影响储存稳定性，相当于提高乳液的保质期。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。
Claims (10)
1.一种红外反射乳液的制备方法，其特征在于，所述方法包括：
对红外反射粒子进行表面修饰，使其表面获得反应活性；
将修饰后的红外反射粒子与单体乳液聚合，使其负载于乳液胶粒。
2.根据权利要求1所述的一种红外反射乳液的制备方法，其特征在于，所述红外反射粒子粒径为亚微米级，所述红外反射粒子表面存在羟基。
3.根据权利要求2所述的一种红外反射乳液的制备方法，其特征在于，所述红外反射粒子粒径不超过500纳米，所述红外反射粒子包括氧化锡锑、二氧化钛和二氧化硅中的一种或几种。
4.根据权利要求3中所述的一种红外反射乳液的制备方法，其特征在于，所述对红外反射粒子进行表面修饰具体包括：
将红外反射粒子加入到乙醇中进行脉冲超声分散，加入氨水调节 pH 至弱碱性，添加匹配官能团的偶联剂，加热到预设温度，保温至反应完成后润洗分离即可；
所述偶联剂包括钛酸酯偶联剂、硅烷偶联剂中的一种或几种。
5.根据权利要求1中所述的一种红外反射乳液的制备方法，其特征在于，所述单体包括丙烯酸酯类单体、苯乙烯单体、丙烯酸单体中的一种或几种，所述丙烯酸酯类单体包括丙烯酸正丁酯、丙烯酸乙酯中的一种或几种。
6.根据权利要求5中所述的一种红外反射乳液的制备方法，其特征在于，所述将修饰后的红外反射粒子与单体乳液聚合具体包括：
将单体、修饰后的红外反射粒子加入到含有乳化剂、引发剂的水溶液中，充分分散后，通入氮气除去氧气，在预定温度下反应，并通过搅拌提供剪切力，反应结束后加入聚乙二醇，并调节乳液体系 pH。
7.根据权利要求6中所述的一种红外反射乳液的制备方法，其特征在于，所述乳液体系中单体含量为2-60 wt％，乳液体系调节后的pH值大于7。
8.根据权利要求7中所述的一种红外反射乳液的制备方法，其特征在于，所述乳化剂为阴离子乳化剂和非离子乳化剂组成的复配乳化剂，且阴离子乳化剂和非离子乳化剂的质量比为 3:1-6。
9.根据权利要求8中所述的一种红外反射乳液的制备方法，其特征在于，所述阴离子乳化剂为十二烷基苯磺酸钠，所述非离子乳化剂为壬基酚聚氧乙烯醚，所述水溶液中的水为去离子水且电导率≤25μS/cm。
10.根据权利要求6中所述的一种红外反射乳液的制备方法，其特征在于，所述单体预先进行纯化去阻聚剂处理，所述引发剂预先进行纯化去除稳定剂处理；
所述充分分散为采用超声分散，并在分散时使用冰水浴控制超声温度不超过10℃。
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