CN112940536B - 一种兼具高近红外反射率和变色效果的无机功能色料及其制备与应用 - Google Patents
一种兼具高近红外反射率和变色效果的无机功能色料及其制备与应用 Download PDFInfo
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Abstract
本发明公开了一种兼具高近红外反射率和变色效果的无机功能色料及其制备与应用。所述方法为:(1)按照钕元素与钼元素的摩尔比为8:5~20:11,称取含钕原料和含钼原料,加水配成浆料并进行湿法研磨,干燥,破碎,得到钕钼混合物;(2)将钕钼混合物进行高温煅烧,破碎,得到无机功能色料。本发明制备方法工艺简单,原料物理化学性质安全,便于工业化。本发明所得色料兼具高近红外反射和变色效果。
Description
技术领域
本发明属于玻璃、陶瓷色釉料以及涂料领域,具体涉及一种兼具高近红外反射率和变色效果的无机功能色料及其制备与应用。
背景技术
变色色料是一种新型色料,其变色效果通过稀土掺杂实现。钕、铒等镧系稀土离子的4f电子具有独特的光谱特性,使离子在可见光范围内产生多条强吸收谱线,将光谱分为若干反射带和吸收带。不同光源之间的能量分布存在差异,经过上述反射带和吸收带的加权后,差异被放大,产生了变色效应。已公开技术中,提供了焦硅酸钕变色色料的制备方法。部分焦硅酸钕色料通过成分调控,兼具高近红外反射率,可反射大部分近红外波段阳光,具有良好的隔热作用。在建筑外墙、汽车车身上使用该色料,可以起到变色装饰效果,也可以有效降低建筑、汽车内的制冷能耗,缓解城市热岛效应。因此兼具变色效果和高近红外反射率的色料具有实际应用价值。
现有技术可以制备出钼钕变色色料,具有不同于焦硅酸钕色料的变色效果。制备的工艺包含介质搅拌磨机械激活和矿化剂辅助合成;并且部分原料溶于水,研磨期间难以保持配料比例;矿化剂可能引起掺杂。
发明内容
为解决现有技术的缺点和不足之处,本发明的首要目的在于提供一种兼具高近红外反射率和变色效果的无机功能色料的制备方法。
本发明不需进行机械激活,设备要求低,稀土元素用量更少,全部采用水溶性弱的原料,无需矿化剂,制备的钼钕色料兼具高近红外反射率和变色效果。
本发明的另一目的在于提供上述方法制得的一种兼具高近红外反射率和变色效果的无机功能色料。
本发明的再一目的在于提供上述一种兼具高近红外反射率和变色效果的无机功能色料的应用。
本发明目的通过以下技术方案实现:
一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,包括以下步骤:
(1)按照钕元素与钼元素的摩尔比为8:5~20:11,称取含钕原料和含钼原料,加水配成浆料并进行湿法研磨,干燥,破碎,得到钕钼混合物;
(2)将钕钼混合物进行高温煅烧,破碎,得到无机功能色料。
优选的,步骤(1)所述含钕原料为氧化钕、氢氧化钕和碳酸钕中的至少一种。
优选的,步骤(1)所述含钼原料为三氧化钼和钼酸中的至少一种。
优选的,步骤(1)所述浆料的固含量为20~30wt.%。
优选的,步骤(1)所述湿法研磨的时间为1~3小时。
优选的,步骤(1)所述干燥的温度为80~120℃,干燥的时间为18~24小时。
优选的,步骤(2)所述煅烧的温度为800~1200℃,更优选为1000~1200℃,时间为3~5小时。
优选的,步骤(2)所述煅烧的升温速率为5~10℃/min。
上述方法制得的一种兼具高近红外反射率和变色效果的无机功能色料。
本发明所得无机功能色料的主要成分为Nd20Mo11O63,属于立方晶系。
上述一种兼具高近红外反射率和变色效果的无机功能色料的应用。
优选的,所述兼具高近红外反射率和变色效果的无机功能色料在建筑外墙、汽车领域中的应用。
与现有技术相比,本发明具有以下优点及有益效果:
(1)变色效果明显,在太阳光下呈灰色,在白炽灯下呈紫色,在荧光灯下呈绿色;(2)近红外反射率高达82%,兼具隔热作用和变色装饰效果;(3)原料易得,设备要求低,工艺流程少,产品容易合成,有利于工业化应用;(4)原料无毒性,不溶于水,不涉及酸碱性溶液及有机液体操作,安全性好。
附图说明
图1为本发明实施例1所得样品的X射线衍射(XRD)图谱,主晶相为Nd20Mo11O63。
图2为实施例1在近红外波段的漫反射光谱。
图3为对比例1在近红外波段的漫反射光谱。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。
本发明实施例中未注明具体条件者,按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等,均为可以通过市售购买获得的常规产品。
实施例1
称取氧化钕136.0克和三氧化钼64.0克,加入800毫升水,采用湿法研磨1小时,得到料浆。
将料浆置于鼓风干燥箱中干燥18小时,干燥温度设定为100℃。
取出干燥物料并破碎,然后将干物料置入箱式电炉,按照升温速率5℃/min,设定升温时间,设定煅烧温度1100℃,保温时间3小时。
待电炉冷却后再经过破碎,可得到兼具变色效果和高近红外反射率的色料,在太阳光下呈灰色,在白炽灯下呈紫色,在荧光灯下呈绿色,近红外反射率81%以上。
实施例2
称取氢氧化钕71.1克和三氧化钼28.9克,加入400毫升水,采用湿法研磨3小时,得到料浆。
将料浆置于鼓风干燥箱中干燥24小时,干燥温度设定为100℃。
取出干燥物料并破碎,然后将干物料置入箱式电炉,按照升温速率7.5℃/min,设定升温时间,设定煅烧温度1000℃,保温时间4小时。
待电炉冷却后再经过破碎,可得到兼具变色效果和高近红外反射率的色料,在太阳光下呈灰色,在白炽灯下呈紫色,在荧光灯下呈绿色,近红外反射率81%以上。XRD图谱与实施例1类似。
实施例3
称取碳酸钕74.7克和三氧化钼25.3克,加入400毫升水,采用湿法研磨2小时,得到料浆。
将料浆置于鼓风干燥箱中干燥20小时,干燥温度设定为100℃。
取出干燥物料并破碎,然后将干物料置入箱式电炉,按照升温速率10℃/min,设定升温时间,设定煅烧温度1200℃,保温时间3小时。
待电炉冷却后再经过破碎,可得到兼具变色效果和高近红外反射率的色料,在太阳光下呈灰色,在白炽灯下呈紫色,在荧光灯下呈绿色,近红外反射率81%以上。XRD图谱与实施例1类似。
实施例4
称取氧化钕66.1克和钼酸38.1克,加入450毫升水,采用湿法研磨3小时,得到料浆。
将料浆置于鼓风干燥箱中干燥18小时,干燥温度设定为100℃。
取出干燥物料并破碎,然后将干物料置入箱式电炉,按照升温速率10℃/min,设定升温时间,设定煅烧温度1200℃,保温时间3小时。
待电炉冷却后再经过破碎,可得到兼具变色效果和高近红外反射率的色料,在太阳光下呈灰色,在白炽灯下呈紫色,在荧光灯下呈绿色,近红外反射率81%以上。XRD图谱与实施例1类似。
对比例1
称取氧化钕141克和三氧化钼59克,加入800毫升水,采用湿法研磨1小时,得到料浆。
将料浆置于鼓风干燥箱中干燥24小时,干燥温度设定为90℃。
取出干燥物料并破碎,然后将干物料置入箱式电炉,按照升温速率5℃/min,设定升温时间,设定煅烧温度1100℃,保温时间3小时。
待电炉冷却后再经过破碎,可得到兼具变色效果和高近红外反射率的色料,主要成分为Nd2MoO6,在太阳光下呈淡紫色,在白炽灯下呈紫色,在荧光灯下呈淡蓝色,近红外反射率74%。
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。
Claims (7)
1.一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,其特征在于,包括以下步骤:
(1)按照钕元素与钼元素的摩尔比为8:5~20:11,称取含钕原料和含钼原料,加水配成浆料并进行湿法研磨,干燥,破碎,得到钕钼混合物;
(2)将钕钼混合物进行高温煅烧,破碎,得到无机功能色料;
步骤(1)所述含钕原料为氧化钕、氢氧化钕和碳酸钕中的至少一种;所述含钼原料为三氧化钼和钼酸中的至少一种。
2.根据权利要求1所述一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,步骤(1)所述浆料的固含量为20~30 wt.%。
3.根据权利要求1所述一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,步骤(2)所述煅烧的温度为800~1200℃,时间为3~5小时。
4.根据权利要求1所述一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,步骤(1)所述湿法研磨的时间为1~3小时。
5.根据权利要求1所述一种兼具高近红外反射率和变色效果的无机功能色料的制备方法,步骤(1)所述干燥的温度为80~120℃,干燥的时间为18~24小时;步骤(2)所述煅烧的升温速率为5~10℃/min。
6.权利要求1~5任一项所述方法制得的一种兼具高近红外反射率和变色效果的无机功能色料。
7.权利要求6所述一种兼具高近红外反射率和变色效果的无机功能色料的应用,其特征在于,在建筑外墙、汽车领域中的应用。
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CN108794005B (zh) * | 2018-06-06 | 2021-03-30 | 华南理工大学 | 一种近红外高反射率功能陶瓷色料及其制备方法 |
CN108929033A (zh) * | 2018-07-17 | 2018-12-04 | 华南理工大学 | 一种具有变色效应的陶瓷玻璃色料及其制备方法 |
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