CN112048193B - 一种兼顾低明度和高近红外反射率的绿色颜料及其制备方法 - Google Patents

一种兼顾低明度和高近红外反射率的绿色颜料及其制备方法 Download PDF

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CN112048193B
CN112048193B CN202010907527.8A CN202010907527A CN112048193B CN 112048193 B CN112048193 B CN 112048193B CN 202010907527 A CN202010907527 A CN 202010907527A CN 112048193 B CN112048193 B CN 112048193B
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陆海鹏
王真雄
温开怀
张珊
朱亚光
翁小龙
邓龙江
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Abstract

本发明属于复合无机颜料技术领域，具体涉及一种兼顾低明度和高近红外反射率的绿色颜料及其制备方法。本发明以三氧化二铬为基料，掺杂二氧化锰通过固相法制备；二氧化锰与氧化铬在高温下发生固溶反应生成尖晶石结构的铬酸锰次相，最终制得的绿色颜料兼顾低明度和高近红外反射率，颜料在可见光波段呈绿色，明度值为24～33；颜料在800～2500nm范围内具有较高的反射率，能作为“冷颜料”应用于热反射涂料中，以及军事伪装材料领域。在深色节能涂层的研究及应用具有广阔的前景。固相合成法制备工艺成熟简单，投入少，便于操作，适合工业化生产。

Description

一种兼顾低明度和高近红外反射率的绿色颜料及其制备方法
技术领域
本发明属于复合无机颜料技术领域，具体涉及一种兼顾低明度和高近红外反射率的绿色 颜料及其制备方法。
背景技术
在酷热的夏季，建筑物、汽车、油罐等因长时间暴露于太阳的照射下，其外表和内部温 度过高，严重影响了人们住行条件的舒适性和工业设施的安全性。构建能够有效地减少空调 系统热负荷和工业设施外表面温度的隔热系统，是目前节能降温设计的一个重要途径。白色 或浅色因其天然对太阳光具有良好的反射作用，被广泛应用于节能建筑和贮藏罐中，然而由 于其耐污性较差以及对颜色的要求，往往需要深色涂料也要具备较好的热反射效果。通过研 制具有红外反射功能的深色颜料，将其添加到涂料中，可制备出具有反射隔热功能的产品。 将其应用于建筑物、屋顶外表以及汽车、船舶、贮藏罐的外壳涂层等方面，可起到良好的隔 热作用。
氧化铬绿颜料具有稳定性好、耐酸碱、耐高温、耐光耐候等优点，常用于油漆、涂料、 陶瓷、玻璃等领域。此外氧化铬绿在可见光波段还具有近似于植物叶片叶绿素的色泽，使其 可用于配制类似绿色叶片的伪装涂料，在高光谱军事探测领域就有科研工作者将铬绿用作伪 装涂层的颜料成分，制得的涂层在400～1300nm波段都能很好的模拟植物叶片的反射光谱。 然而未掺杂的铬绿在近红外波段(780～2500nm)反射率偏低，而叶绿素在近红外波段的反射 率则较高。为此，需开发一种绿色伪装颜料，使其不仅在可见光波段的颜色与叶绿素接近， 而且在近红外波段也要达到叶绿素那样高的反射率。在保持铬绿颜料绿色调的同时提高其在 近红外波段的反射率不仅可用于军事伪装材料领域，用作建筑领域的“冷颜料”也具有重要 的意义。
以氧化铬基为主体，通过掺杂离子来改善其颜色及近红外反射性能是当前研究工作的主 要方法，现有研究有单掺杂、二元掺杂以及多元共掺杂，掺杂的离子有铝离子、钛离子、钴 离子、铁离子、镁离子等。但这些研究结果都未能实现提高近红外波段的反射率的同时还能 保持铬绿颜料绿色调，比如研究表明单掺杂铝离子或钛离子能使铬绿在近红外波段的反射率 达到80％以上，但同时也会使铬绿在可见光的反射率和明度值大幅提高，难以保持铬绿颜料 的绿色调。
发明内容
针对上述存在问题或不足，本发明提供了一种兼顾低明度和高近红外反射率的绿色颜料 及其制备方法，所制备的绿色颜料是一种以三氧化二铬为主相，通过单掺杂二氧化锰制备而 成的无机颜料。能在保持明度值变化不大的条件下获得较高的近红外反射率，满足涂层对颜 色和隔热的要求。
本发明的技术方案如下：
一种兼顾低明度和高近红外反射率的绿色颜料，是一种氧化铬基颜料，其基料为三氧化 二铬，掺杂二氧化锰通过固相法制备，各组分的质量百分比含量为：三氧化二铬75～95％， 二氧化锰5～25％；该绿色颜料的主相为三氧化二铬，次相为尖晶石结构的铬酸锰。
上述绿色颜料的制备方法，包括以下步骤：
步骤1、按照质量百分数称取75～95％的三氧化二铬和5～25％的二氧化锰进行配料。
步骤2、将步骤1所准备的原料加入球磨罐，采用乙醇作为球磨介质，进行湿法球磨将颜 料分散均匀。
步骤3：将步骤2球磨过后的浆料，烘干后进行研磨，过100～200目筛，防止粉料烧结 后结块。
步骤4、固相合成：将步骤3研磨过后的粉料放入马沸炉中烧结，进行固相合成反应，从 室温开始以升温速率4～10℃/min，逐渐升温至900～1300℃后保温2～4小时，再自然冷却 降至室温。
步骤5、二次研磨、过筛：将步骤4固相合成的反应物研磨过100～200目网筛，即可得 到兼顾低明度和高近红外反射率的绿色颜料。
二氧化锰是一种常温下非常稳定的黑色粉末状固体，难溶于水、弱酸、弱碱、硝酸、冷 硫酸，其常作为催化剂或者电池电极材料掺杂应用。本发明首次选用二氧化锰对铬绿进行单 掺杂改性研究：二氧化锰与氧化铬在高温下发生固溶反应生成尖晶石结构的铬酸锰次相，最 终制得的绿色颜料兼顾低明度和高近红外反射率，颜料在可见光波段呈绿色，明度值为24～ 33；颜料在800～2500nm范围内具有较高的反射率，能作为“冷颜料”应用于热反射涂料中， 以及军事伪装材料领域。在深色节能涂层的研究及应用具有广阔的前景。固相合成法制备工 艺成熟简单，投入少，便于操作，适合工业化生产。
附图说明
图1为实施例颜料在400～2500nm范围内的反射光谱。
具体实施方式
下面通过实施例和附图对本发明作进一步说明，但本发明并不限于以下实施例。
实施例1
按照质量百分比称取以下原料：三氧化二铬，29.14g；二氧化锰，0.86g；再按球：料： 乙醇＝4:1:1称取锆球，120g；乙醇，30g一起加入球磨罐，以乙醇为球磨介质，采用行星式 湿法球磨混合均匀，烘干研磨，过100目筛去除大颗粒，然后置于马沸炉内进行固相反应。 从室温逐渐升至1200℃，保温后随炉冷却至室温。最后将粉体研磨过筛，制得绿色颜料S1。
实施例2
按照质量百分比称取以下原料：三氧化二铬，28.29g；二氧化锰，1.71g；再按球：料： 乙醇＝4:1:1称取锆球，120g；乙醇，30g一起加入球磨罐，以乙醇为球磨介质，采用行星式 湿法球磨混合均匀，烘干研磨，过100目筛去除大颗粒，然后置于马沸炉内进行固相反应。 从室温逐渐升至1200℃，保温后随炉冷却至室温。最后将粉体研磨过筛，制得绿色颜料S2。
实施例3
按照质量百分比称取以下原料：三氧化二铬，26.61g；二氧化锰，3.38g；再按球：料： 乙醇＝4:1:1称取锆球，120g；乙醇，30g一起加入球磨罐，以乙醇为球磨介质，采用行星式 湿法球磨混合均匀，烘干研磨，过100目筛去除大颗粒，然后置于马沸炉内进行固相反应。 从室温逐渐升至1200℃，保温后随炉冷却至室温。最后将粉体研磨过筛，制得绿色颜料S3。
实施例4
按照质量百分比称取以下原料：三氧化二铬，25.78g；二氧化锰，4.22g；再按球：料： 乙醇＝4:1:1称取锆球，120g；乙醇，30g一起加入球磨罐，以乙醇为球磨介质，采用行星式 湿法球磨混合均匀，烘干研磨，过100目筛去除大颗粒，然后置于马沸炉内进行固相反应。 从室温逐渐升至1200℃，保温后随炉冷却至室温。最后将粉体研磨过筛，制得绿色颜料S4。
以上所有实施例的球磨速度为250r/min，球磨时间2.5小时；升温速率5℃/min，保温 时间3小时。
分别取适量实施例1、2、3、4制得的颜料样品以及纯三氧化二铬装入粉末样品杯，用分 光光度计测量各颜料样品的可见光及近红外反射率，如图1所示。
采用精密色差计对实施例1、2、3、4和纯三氧化二铬进行测量，结果如表1所示。
表1实施例色度坐标值(实施例1、2、3、4和纯三氧化二铬的颜色参数)
Figure BDA0002661977190000031
L表示明度，a*表示从绿色至红色的范围，b*表示从蓝色至黄色的范围。当二氧化锰掺杂 量为20％时，该颜料在可见光波段呈绿色且明度值低于30，同时在近红外波段范围的平均反 射率达到84％。
综上可见，本发明首次选用二氧化锰对铬绿进行单掺杂改性研究：二氧化锰与氧化铬在 高温下发生固溶反应生成尖晶石结构的铬酸锰次相，最终制得的绿色颜料兼顾低明度和高近 红外反射率，颜料在可见光波段呈绿色，明度值为24～33，具体颜色参数见表1；颜料在800～ 2500nm范围内具有较高的反射率，能作为“冷颜料”应用于热反射涂料中(见附图1)。在深 色节能涂层的研究及应用具有广阔的前景。固相合成法制备工艺成熟简单，投入少，便于操 作，适合工业化生产。

Claims (3)

1.一种兼顾低明度和高近红外反射率的绿色颜料，其特征在于：是一种氧化铬基颜料，其基料为三氧化二铬，掺杂二氧化锰通过固相法制备，各组分的质量百分比含量为：三氧化二铬75～95％，二氧化锰5～25％；该绿色颜料的主相为三氧化二铬，次相为尖晶石结构的铬酸锰。
2.如权利要求1所述兼顾低明度和高近红外反射率的绿色颜料，其制备方法，包括以下步骤：
步骤1、按照质量百分数称取75～95％的三氧化二铬和5～25％的二氧化锰进行配料；
步骤2、将步骤1所准备的原料加入球磨罐，采用乙醇作为球磨介质，进行湿法球磨将颜料分散均匀；
步骤3、将步骤2球磨过所得的浆料，烘干后进行研磨，过100～200目筛；
步骤4、将步骤3研磨过后的粉料放入马沸炉中烧结，进行固相合成反应，从室温开始以升温速率4～10℃/min，升温至900～1300℃后保温2～4小时，再自然冷却降至室温；
步骤5、将步骤4固相合成的反应物研磨过100～200目网筛，即可得到兼顾低明度和高近红外反射率的绿色颜料。
3.一种兼顾低明度和高近红外反射率的绿色颜料，其特征在于：应用于建筑领域作为冷颜料或军事伪装材料领域。
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