CN111944355A - 一种氟碳涂料改性剂的制备方法、制备及其应用 - Google Patents
一种氟碳涂料改性剂的制备方法、制备及其应用 Download PDFInfo
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Abstract
本发明公开了一种氟碳涂料改性剂的制备方法、制备及其应用,通过采用煅烧法将三聚氰胺和淀粉的混合物进行多步煅烧,获得淀粉/g‑C3N4;之后按质量比5:1‑10:1的比例将淀粉/g‑C3N4粉末和溶于无水乙醇的硅烷偶联剂溶于水中,在PH为4‑5的酸性条件下回流加热反应得到硅烷改性淀粉/g‑C3N4。并将所制备的硅烷改性淀粉/g‑C3N4应用于水性氟碳涂料中。通过将本发明所制备的具有可见光催化性能的硅烷改性淀粉/g‑C3N4加入到氟碳涂料中,相比传统的氟碳涂料可见光催化能力提高了20%~40%,明显得提高氟碳涂料自清洁能力。
Description
技术领域
本发明属于涂料材料领域,具体涉及一种氟碳涂料改性剂的制备方法、制备及其应用。
背景技术
水性氟碳涂料是一种比较新的工业材料,具有较好的防粘性能、易洗刷且具有良好的稳定性和耐候性,是一种优秀的新型涂料。现在已经广泛应用于建筑领域,其代表性建筑有首都机场航站楼、东方明珠电视塔和郑州国际会展中心等。
现有水性氟碳涂料虽然具有良好的耐候性,但是其所使用关键颜料氟碳乳液具有疏水亲油性,在使用过程中难免受到有机物及细菌的污染,若清洗将会投入大量的人力物力,而且清洗效果较差,这样会导致装饰效果较差而限制了涂料的应用。
现有技术中主要采用两种方式提高氟碳涂料自清洁能力。方法一:提高涂料的疏水性:超疏水涂料能够利用雨水冲走污染物而实现自清洁效果,该类涂料的自清洁效果较差,清洗需要耗费大量的人力及物力。方法二:光催化机理,通过利用二氧化钛为光催化剂进行光催化清洁,但是由于二氧化钛的吸收光区主要在紫外光,故其自清洁效果有限。
发明内容
针对现有技术中水性氟碳涂料自清洁效果差的问题,本发明提出一种可见光催化自清洁性能的氟碳涂料改性剂,给出了该改性剂的制备方法并将其应用到水性氟碳涂料中。
实现上述技术目的,达到上述技术效果,本发明通过以下技术方案实现:
一种氟碳涂料改性剂的制备方法的制备方法,包括以下步骤:
步骤一:采用煅烧法将三聚氰胺和淀粉的混合物进行多步煅烧,获得淀粉/g-C3N4;
步骤二:按质量比5:1-10:1的比例将淀粉/g-C3N4粉末和溶于无水乙醇的硅烷偶联剂溶于水中,在PH为4-5的酸性条件下回流加热反应得到硅烷改性淀粉/g-C3N4。
作为本发明的进一步改进,步骤二,所述的回流加热反应的反应温度为70~90℃,反应时间为4~5h。
作为本发明的进一步改进,步骤二,在反应溶液体系中,所述淀粉/g-C3N4的浓度为3.64g/L~5.45g/L,所述硅烷偶联剂的浓度为0.54g/L~1.09g/L。
作为本发明的进一步改进,所选用的硅烷偶联剂在无水乙醇的浓度为4g/L~10g/L。
作为本发明的进一步改进,步骤一,淀粉/g-C3N4的具体步骤为:
在超声的条件下,将三聚氰胺和淀粉按20:1-25:1的比例分散在水溶液中,之后水浴烘干,或者分散均匀的三聚氰胺和淀粉的混合物;
将所获得混合物放入煅烧炉中,在高于600℃的条件下煅烧1.5-2.5h,之后将煅烧的固体研磨后至一定的细度,再次煅烧。
作为本发明的进一步改进,步骤一中,经研磨和二次煅烧后选取粒径小于200目的淀粉/g-C3N4粉末的用于步骤二的制作。
本发明还提供了一种根据以上所述的制备方法制备的氟碳涂料改性剂。
本发明还提供了一种将以上所述的改性剂在氟碳涂料中的应用,所述的改性剂在氟碳涂料中所占质量比为0.2%-1%。
本发明的有益效果:通过采用本发明的方法所制备的光催化剂核心离子在可见光区具有较强的光催化性能,进一步所制备的硅烷改性淀粉/g-C3N4在保留光催化性能的基础上通过改性处理提高了其应用于氟碳涂料中的相容性的作用,加入了该改性光催化剂的氟碳涂料中,相比传统的氟碳涂料可见光催化能力提高了20%~40%,明显得提高氟碳涂料自清洁能力较强。
附图说明
图1为所制备的淀粉/g-C3N4的紫外可见光的吸收光谱图;
图2为所制备的硅烷改性淀粉/g-C3N4的紫外可见光的吸收光谱图;
图3为所制备的淀粉/g-C3N4的XRD图;
图4为所制备的硅烷改性淀粉/g-C3N4的吸光度图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
(1)制备淀粉/g-C3N4粉末:首先采用电子天平称取10g的三聚氰胺溶解于100ml水中,充分搅拌,然后分别加入0.5g淀粉,超声分散20分钟,在水浴锅中蒸干,取出粉末在研钵中进行研磨30min,放入到马弗炉中,以5℃/min升温速率升温到600℃,在600℃恒温2h后取出,进一步研磨,待均匀后放入马弗炉中650℃继续加热2h,然后冷却至室温,过200目筛得到二次加热获得淀粉掺杂g-C3N4。
(2)制备改性剂:将1g淀粉/g-C3N4粉末溶解于200ml水中,使用超声波清洗机超声分散15min,将0.18g硅烷偶联剂KH570分别溶解到20ml无水乙醇中加入,使用醋酸调整pH至4.0,转入三颈烧瓶当中,将装有淀粉/g-C3N4和KH570的三颈烧瓶放到恒温水浴锅,升温至温度80℃,以1000r/min进行磁力搅拌,加热回流5h,待反应结束后通过真空抽滤去除水分,将滤渣在80℃烘干,研磨得到硅烷改性淀粉/g-C3N4。
(3)应用于水性氟碳涂料:将0.2份上述制备的硅烷改性淀粉/g-C3N4粉末加入到33份去离子水中,超声震荡30min,倒入砂磨分散机中,以500r/min进行旋转,依次加入1份丙二醇、0.3份pH调节剂及0.2份消泡剂,搅拌15min,然后加入60份氟碳乳液及4.2份成膜助剂分散十分钟,最后加入0.2份杀菌剂CMC、0.1份增稠剂PUR80和0.2份增稠剂612NC,继续分散十五分钟,完成氟碳涂料的配制。
实施例2:本实施例与实施例1基本一致,不同的是步骤3中,硅烷偶联剂改性淀粉/g-C3N4的加入量为0.4份。
实施例3:本实施例与实施例1基本一致,不同的是步骤3中,硅烷偶联剂改性淀粉/g-C3N4的加入量为0.6份。
实施例4:本实施例与实施例1基本一致,不同的是步骤3中,硅烷偶联剂改性淀粉/g-C3N4的加入量为0.8份。
实施例5:本实施例与实施例1基本一致,不同的是步骤3中,硅烷偶联剂改性淀粉/g-C3N4的加入量为1份。
对比例1:本实施例与实施例1基本一致,不同的是步骤3中,不加入硅烷偶联剂改性淀粉/g-C3N4。
测试方法为:
测试1:紫外-分光光度计表征
采用UV-1601型紫外-分光光度计进行紫外-可见漫反射分析,以硫酸钡为标准物,对淀粉/g-C3N4和硅烷改性淀粉/g-C3N4进行分析测试,检测器狭缝宽度为20nm,测试的波长范围在200-800nm,所获得的紫外可见光的吸收光谱图分别如图1和图2所示。由图1可知制备的淀粉/g-C3N4材料的吸收边在470nm附近,位于可见光区域,当采用硅烷偶联剂改性后吸收边在460nm附近,仍然位于可见光区域。
测试2:XRD表征
采用日本岛津公司生产的XD-3A型半自动X衍射仪(XRD)进行分析,辐射源为Cu-Kα管电压为40kv,于30mA电流下进行扫描,扫描角度范围设置到10°到70°,扫描步长为0.02°,扫描速率为20°/min。所获得的XRD图如图3所示。由图3可以看出所获得的样品衍射峰强且尖锐,说明制备淀粉/g-C3N4具有较好的结晶度。
测试3:分散稳定性测试
由于吸光度和纳米粒子的分散程度呈现正相关关系,吸光度法遵循lamber-Beer’s定律,因此吸光度可以表现其分散稳定程度,具体操作如下:使用移液枪从样品中移出5ml硅烷改性淀粉/g-C3N4浆液,装入比色皿中,使用紫外-可见分光光度计在553nm处测量其吸光度,由图4可以看出获得样品的分散稳定性得到大幅度提高。
测试4:水性氟碳涂料性能测试
将实施例1-5和对比例1制备的涂料均匀涂覆在混凝土表面,使用色差仪观察颜色变化以及分析,读数根据LAB系统得出L、a和b的比色参数,L表示由黑色到白色的亮度值,a表示由绿色到红色的值,b表示由黄色到蓝色的值,手持色差仪测定每个水泥板样品的表面作为背底,测试样品中表面取三个不同的点,然后将配置好的10mg/L的将罗丹明B溶液滴入到氟碳涂层的表面,通过可见光进行照射,用色差仪测定各个Lab的值,根据公式△E=(△L)2+(△a)2+(△b)2从而计算出每个样品的色差,通过公式R△E(t)=(△E(0)-△E(t))/△E(0)来计算样品在24h可见光照射的降解率,如表1所示。
表1:不同实施例的涂料Rhb降解率
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (8)
1.一种氟碳涂料改性剂的制备方法的制备方法,其特征在于,包括以下步骤:
步骤一:采用煅烧法将三聚氰胺和淀粉的混合物进行多步煅烧,获得淀粉/g-C3N4;
步骤二:按质量比5:1-10:1的比例将淀粉/g-C3N4粉末和溶于无水乙醇的硅烷偶联剂溶于水中,在PH为4-5的酸性条件下回流加热反应得到硅烷改性淀粉/g-C3N4。
2.根据权利要求1所述的制备方法,其特征在于:步骤二,所述的回流加热反应的反应温度为70~90℃,反应时间为4~5 h。
3.根据权利要求1所述的制备方法,其特征在于:步骤二,在反应溶液体系中,所述淀粉/g-C3N4的浓度为3.64g/L~5.45g/L,所述硅烷偶联剂的浓度为0.54 g/L~1.09g/L。
4.根据权利要求3所述的制备方法,其特征在于:所选用的硅烷偶联剂在无水乙醇的浓度为4g/L~10g/L。
5.根据权利要求1所述的制备方法,其特征在于:步骤一,淀粉/g-C3N4的具体步骤为:
在超声的条件下,将三聚氰胺和淀粉按20:1-25:1的比例分散在水溶液中,之后水浴烘干,或者分散均匀的三聚氰胺和淀粉的混合物;
将所获得混合物放入煅烧炉中,在高于600℃的条件下煅烧1.5-2.5h,之后将煅烧的固体研磨后至一定的细度,再次煅烧。
6.根据权利要求5所述的制备方法,其特征在于:步骤一中,经研磨和二次煅烧后选取粒径小于200目的淀粉/g-C3N4粉末的用于步骤二的制作。
7.根据权利要求1-6任一所述的制备方法制备的氟碳涂料改性剂。
8.以权利要求7所述的改性剂在氟碳涂料中的应用,其特征在于:所述的改性剂在氟碳涂料中所占质量比为0.2%-1%。
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