CN111057399B - 一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法 - Google Patents

一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法 Download PDF

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CN111057399B
CN111057399B CN202010110677.6A CN202010110677A CN111057399B CN 111057399 B CN111057399 B CN 111057399B CN 202010110677 A CN202010110677 A CN 202010110677A CN 111057399 B CN111057399 B CN 111057399B
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王爱勤
王晓雯
牟斌
汪琴
许江
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明提供了一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，是将稀土元素水合盐、铋盐充分溶解于硝酸溶液中形成溶液A；将钒盐及黏土矿物搅拌溶解分散于硝酸或氢氧化钠溶液形成悬浮液B；然后将溶液A滴加到悬浮液B中，再加入pH调节剂调节混合液pH至6~8，搅拌反应0.5~3h；反应产物经离心洗涤至中性后经煅烧，粉碎，得稀土掺杂黏土矿物基铋黄杂化颜料。本发明通过引入黏土矿物实现了铋黄杂化颜料粒径和粒径分布的调控，同时有效降低了高档铋黄颜料的制备成本；通过引入稀土元素和黏土矿物制备的铋黄杂化颜料具有荧光可调性能；采用化学沉淀法制备稀土掺杂黏土矿物基铋黄杂化颜料，操作简单、方便，可控性强。

Description

一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的 制备方法
技术领域
本发明涉及一种稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，尤其涉及一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，属于环保型无机颜料技术领域。
背景技术
黄色的光波范围为565~595 nm，处于人们眼球对光最敏感的波段（400 ~ 700nn）。因此，作为高能见度警示色颜料的黄色无机颜料，被广泛应用于交通、道路、起重机械等需要人们高度醒目的地方。在众多黄色无机颜料中，铋黄颜料（BiVO4）在450 nm处反射率明显高于其它颜料，是一种性能优异的环保型黄色无机颜料。但由于铋黄颜料价格昂贵，且在热处理工序时不可避免会造成晶粒生长和团聚。研究表明，通过引入载体材料可显著改善无机纳米粒子的团聚现象，尤其是通过引入天然黏土矿物制备的环保型杂化无机颜料，不仅有效改善了无机纳米颜料的团聚现象，同时大幅降低了环保型无机颜料的生产成本。
稀土元素性质活泼，具有独特的4f电子结构，其离子态多呈现三价，且离子半径范围为0.84 ~1.06Å。稀土钒酸盐纳米材料集稀土钒酸盐独特的电子结构、强自旋轨道效应和大的原子磁矩等特性和纳米特性于一体，在陶瓷、发光材料、催化剂、环保材料等领域具有良好应用前景。此外，Bi3+与稀土离子价态相同，且离子半径相近，所以稀土元素常被作为掺杂元素制备稀土掺杂的钒酸铋，制得产物具有良好发光、光催化产氢性能。Starsich等人合成的BiVO4: Nd3+可以在20 mm的深度观察到荧光纳米颗粒，且荧光纳米颗粒具有空间分辨率好、光稳定性高等特点（Chem. Mater. 2017, 29, 8158-8166）。目前，稀土掺杂钒酸铋材料研究主要集中于光催化领域，但稀土掺杂对钒酸铋颜料颜色的影响规律鲜有研究。Sameera等人采用常规固相反应制备了Li0.10RE0.10Bi0.8Mo0.2V0.8O4 (RE = La, Pr, Sm, Gd,Tb, Dy, Y, Yb, Lu)高反射率黄色无机颜料，但并未考察稀土掺杂量对铋黄颜料色度的影响（ACS Sustainable Chem. Eng. 2015, 3, 1227−1233）。众所周知，材料的带隙能与其颜色之间存在一定的关系，采用不同量、不同稀土元素掺杂容易引起钒酸铋晶格的变形及扭曲，从而导致钒酸铋导带与价带的之间能量差（即带隙能）发生变化，最终实现对其色度的调控，可被潜在地应用于发光材料领域。
发明内容
本发明的目的是针对现有铋黄颜料制备技术缺陷和颜色性能需求，提供一种化学沉淀法制备稀土掺杂黏土矿物基铋黄杂化颜料的方法，开发具有荧光和颜色可调的铋黄颜料制备技术。
一、稀土掺杂黏土矿物基铋黄杂化颜料的制备
将稀土元素水合盐、铋盐充分溶解于硝酸溶液（浓度1~8mol/L）中形成溶液A；将钒盐及黏土矿物搅拌溶解分散于硝酸溶液（浓度1~8mol/L）或氢氧化钠溶液（浓度1~8mol/L）中形成浅黄色悬浮液B；然后将溶液A滴加到悬浮液B中，再加入pH调节剂调节混合液pH至6~8，搅拌反应0.5~3h；反应产物经离心洗涤至中性后在300~800ºC煅烧0.5~4h，粉碎，过筛，制得稀土掺杂黏土矿物基铋黄杂化颜料。
所述稀土元素水合盐为硝酸铕、硝酸钆、硝酸铈、硝酸钐、硝酸镧、氯化铕、氯化钆、氯化铈、氯化钐、氯化镧、醋酸铕、醋酸钆、醋酸铈、醋酸钐和醋酸镧中的至少一种。所述铋源为氧化铋、硝酸铋、氯化铋、醋酸铋或者硫酸铋中的至少一种。稀土元素水合盐与铋源的物质的量之比为0.005~0.1:1。
所述钒源为五氧化二钒、偏钒酸铵，偏钒酸钠或者钒酸钠中的至少一种。铋源和掺杂剂物质的量之和与钒源的物质的量之比为1:0.5 ~ 1:5。
所述黏土矿物为凹凸棒石、高岭土、埃洛石、滑石、硅灰石、蒙脱石、海泡石、伊利石中的至少一种，黏土矿物的加入量以其在稀土掺杂铋黄颜料的质量百分含量为10~80%计量。
所述pH调节剂为氨水、氢氧化钠、氢氧化钾、磷酸钠、磷酸一氢钠、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾中的至少一种。
二、稀土掺杂黏土矿物基铋黄杂化颜料的结构和性能表征
1、X-射线衍射谱图
图1为本发明制备的铋黄颜料的X-射线衍射谱图。如图所示，在2θ = 18.681°、18.989°、28.921°、30.531°、34.511°、35.201°、39.561°、39.781°、40.050°和42.470°处出现了单斜白钨矿型BiVO4的特征衍射峰，分别对应于（011）、（011）、（112）、（004）、（200）、（020）、（-211）、（211）、（-121）和（015）晶面。对比未掺杂稀土元素的铋黄杂化颜料和没有引入黏土矿物的铋黄颜料的特征峰发生了位移（Appl. Clay Sci. 2019, 181, 105221.），表明引入稀土元素和黏土矿物明显引起了铋黄颜料晶格的畸变，这可能归因于稀土元素和黏土矿物主要元素在高温晶化过程中共掺杂效应。
2、透射电镜分析
图2为本发明制备的La掺杂的埃洛石基铋黄杂化颜料的透射电镜（a、b）和高分辨透射电镜照片（c）。如图a和b所示，钒酸铋颗粒成功负载于管状埃洛石管壁和管内；同时从图2c晶格间距证实其为单斜白钨矿型BiVO4的（-121）晶面。
3、铋黄杂化颜料的颜色性能
本发明实施例1-5制备的铋黄杂化颜料样品的CIE-L * a * b * 颜色参数如表1所示。铋黄杂化颜料的b * 值范围为82.00~90.12之间，且a * 值除H-4样品达到5.32之外，均低于1，特别是对H-3样品甚至达到了-1.13，表明其绿相增强。同时发现五个实例样品的亮度L * 均高于78。对比样品的最大吸收边Kubelka-Munk曲线（图3），从H-1至H-5每个样品的最大吸收边分别为497.66nm、502.00nm、503.01nm、507.53nm和505.02nm，计算可得五个实例样品的带隙能值分别为2.49eV、2.47eV、2.47eV、2.44eV和2.46eV。根据无机颜料的色度与带隙能之间的相关性，通过掺杂元素的掺杂引起钒酸铋的Bi 6s 和O 2p 杂化轨道形成价带与导带之间的能量差，从而导致钒酸铋的色度发生变化。通过以上分析表明，稀土元素的掺杂成功引起黏土矿物基铋黄杂化颜料的色度和带隙能的变化，从而实现了对钒酸铋的色度的成功调控。
综上所述，本发明制备铋黄杂化颜料的方法相对现有技术和产品具有以下优点：
1、通过引入黏土矿物，不仅实现了铋黄杂化颜料粒径和粒径分布的调控，同时有效降低了高档铋黄颜料的制备成本；
2、通过引入稀土元素和黏土矿物，使制备铋黄杂化颜料具有荧光和颜色可调性能，有望用于高速公路警示牌、高档汽车面漆等领域；
3、采用化学沉淀法制备稀土掺杂黏土矿物基铋黄杂化颜料，操作简单、方便，可控性强。
附图说明
图1为本发明制备的稀土掺杂黏土矿物基铋黄杂化颜料的X-射线衍射谱图。
图2为本发明制备的铋黄杂化颜料的透射电镜照片。
图3为本发明制备的铋黄杂化颜料杂化颜料的Kubelka-munk曲线。
具体实施方式
下面通过具体实施例对本发明稀土掺杂黏土矿物基铋黄杂化颜料的制备和性能作进一步说明。
实施例1
将0.483g硝酸铋和0.002g硝酸镧溶于5mol/L的硝酸溶液中形成A溶液；将0.160g偏钒酸钠溶于5mol/L的氢氧化钠溶液，加入0.200g埃洛石，充分搅拌分散均匀形成悬浮液B；然后将A溶液滴加至悬浮液B中，再加入Na2CO3调节pH至6.5后，磁力搅拌1h；产物离心洗涤至中性后，置于100oC烘箱中干燥2h后得到前驱体；最后将前驱体置于马弗炉中，在700ºC煅烧2h；产物经研磨粉碎，过筛，即得镧元素掺杂黏土矿物基铋黄杂化颜料，标记为H-1，其L * 、a * 、b * 颜色参数见表1。
实施例2
将0.284g氯化铋和0.043g硝酸铈溶于2mol/L的硝酸溶液中形成溶液A；将0.5849g偏钒酸铵和0.259g滑石加至2mol/L的硝酸溶液中搅拌溶解、分散0.5h形成悬浮液B，然后将溶液A滴加至悬浮液B，再加入磷酸钠调节pH至7后，继续搅拌3h；离心洗涤至中性，直接置于马弗炉中在300ºC下煅烧4h；产物经粉碎，过筛，得铈元素掺杂滑石/铋黄杂化颜料，样品标记为H-2，其L * 、a * 、b * 颜色参数见表1。
实施例3
将0.352g硫酸铋和0.0007g醋酸铕溶于2mol/L的硝酸溶液中形成溶液A；将0.092g钒酸钠和0.032g高岭土加至8mol/L的氢氧化钠溶液中搅拌溶解分散2h形成悬浮液B；然后将溶液A滴加至悬浮液B，再加入氨水调节pH至8后，继续搅拌1.5h；反应产物离心洗涤至中性后直接置于马弗炉中经800ºC煅烧0.5h，粉碎，过筛，得铕元素掺杂掺杂高岭石基铋黄杂化颜料，样品标记为H-3，其L * 、a * 、b * 颜色参数见表1。
实施例4
将0.387g硝酸铋、0.046g氧化铋和0.001g硝酸钐溶于8mol/L的硝酸溶液中形成溶液A；将0.1117g偏钒酸铵和0.162g海泡石加至4mol/L的硝酸溶液中搅拌溶解、分散1h形成悬浮液B；然后将溶液A滴加至悬浮液B，再加入氢氧化钠调节pH至7，继续搅拌1h；产物离心洗涤至中性后直接置于马弗炉中在600ºC煅烧1h，粉碎，过筛，得钐元素掺杂海泡石/铋黄杂化颜料，样品标记为H-4，其L * 、a * 、b * 颜色参数见表1。
实施例5
将0.314g氯化铋、0.002g硝酸钆溶于1mol/L的硝酸溶液中形成溶液A；将0.113g偏钒酸钠、0.091g五氧化二钒和0.065g蒙脱石加至2mol/L的硝酸溶液中搅拌溶解、分散形成悬浮液B；然后将溶液A滴加至悬浮液B，再加入氨水调节pH至6，继续搅拌3h；产物离心洗涤至中性后直接置于马弗炉中在500ºC煅烧2h，粉碎，过筛，得钆元素掺杂蒙脱石/铋黄杂化颜料，样品标记为H-5，其L * 、a * 、b * 颜色参数见表1。
Figure DEST_PATH_IMAGE001

Claims (7)

1.一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，是将稀土元素水合盐、铋盐充分溶解于硝酸溶液中形成溶液A；将钒盐及黏土矿物搅拌溶解分散于硝酸溶液或氢氧化钠溶液中形成浅黄色悬浮液B；然后将溶液A滴加到悬浮液B中，再加入pH调节剂调节混合液pH至6~8，搅拌反应0.5~3h；反应产物经离心洗涤至中性后在300~800ºC煅烧0.5~4h，粉碎，过筛，制得稀土掺杂黏土矿物基铋黄杂化颜料；
稀土元素水合盐为硝酸铕、硝酸钆、硝酸铈、硝酸钐、硝酸镧、氯化铕、氯化钆、氯化铈、氯化钐、氯化镧、醋酸铕、醋酸钆、醋酸铈、醋酸钐和醋酸镧中的至少一种；稀土元素水合盐与铋源的物质的量之比为0.005~0.1:1；
铋源和稀土元素水合盐物质的量之和与钒源的物质的量之比为1:0.5 ~ 1:5；
黏土矿物的加入量以其在稀土掺杂铋黄颜料的质量百分含量为10~80%计量。
2.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述铋源为氧化铋、硝酸铋、氯化铋、醋酸铋或者硫酸铋中的至少一种。
3.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述钒源为五氧化二钒、偏钒酸铵，偏钒酸钠或者钒酸钠中的至少一种。
4.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述黏土矿物为凹凸棒石、高岭土、埃洛石、滑石、硅灰石、蒙脱石、海泡石、伊利石中的至少一种。
5.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述pH调节剂为氨水、氢氧化钠、氢氧化钾、磷酸钠、磷酸一氢钠、碳酸钠、碳酸钾、碳酸氢钠、碳酸氢钾中的至少一种。
6.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述硝酸溶液的浓度为1~8mol/L。
7.如权利要求1所述一种荧光和颜色可调的稀土掺杂黏土矿物基铋黄杂化颜料的制备方法，其特征在于：所述氢氧化钠溶液的浓度为1~8mol/L。
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