CN1294211C - 超分子结构光热稳定型耐晒艳红bbc颜料及其插层方法 - Google Patents
超分子结构光热稳定型耐晒艳红bbc颜料及其插层方法 Download PDFInfo
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Abstract
本发明介绍了一种超分子结构光热稳定型耐晒艳红BBC颜料及其插层方法。为了提高有机颜料耐晒艳红BBC的耐光性和耐热性，本发明利用水滑石的可插层性，以层间阴离子为NO3 -的水滑石为前体，用离子交换法将耐晒艳红BBC的阴离子插入到水滑石层间，使耐晒艳红BBC的阴离子全部取代水滑石层间的NO3 -，得到的插层水滑石LDH-BBC颜料不但保持了耐晒艳红BBC本身的颜色，而且与耐晒艳红BBC相比，其耐光性和耐热性均有大幅度的提高。该LDH-BBC颜料可代替耐晒艳红BBC广泛用于涂料、油漆和复合材料中。
Description
所属领域：本发明涉及一种超分子结构光热稳定型耐晒艳红BBC颜料及其插层方法。
背景技术：耐晒艳红BBC是一种含有偶氮基团的色淀颜料，由于其耐光、耐热性能差，使其应用范围和使用效果受到了极大的限制，因此提高耐晒艳红BBC的耐光、耐热性能具有十分重要的意义。类水滑石(Layered DoubleHydroxides，简写为LDHs)是一种阴离子型层状材料，由于其具有可插层组装的性能，因而利用此性能可将一些功能物种插入到水滑石层间，制备具有特殊功能的超分子插层结构材料。
文献Mohd Zobir bin Hussein，Zulkarnain Zainal，Asmah Hj.Yahaya，Azirabinti Abd.Aziz，Materials Science and Engineering B88，2002，98-102，将酸性染料萘蓝黑10B的水溶液与含有Mg2+和Al3+的水溶液混合，调整反应体系的pH＝10，得到层间为萘蓝黑10B阴离子的插层水滑石，该插层方法为共沉淀法。其研究的目的只是得到一种无机-有机纳米复合材料，并未考察产物能否作为一种新型颜料来使用。
文献Umberto Costantino，Natascia Coletti，and Morena Nocchetti，Langmuir，1999，15：4454-4460中，先采用尿素热合成法得到水滑石[Zn0.67Al0.33(OH)2][CO3]0.165·0.4H2O，再将其与NaCl和HCl反应得到水滑石Zn0.67Al0.33(OH)2Cl0.33·0.4H2O，再以Zn0.67Al0.33(OH)2Cl0.33·0.4H2O为前体，甲基橙(MO)为客体，组装得到插层水滑石[Zn0.67Al0.33(OH)2][MO0.31Cl0.02]·0.85H2O，他们考察了产物的荧光性。其缺点是前体制备方法复杂。
发明内容：本发明的目的是利用LDHs的可插层性，将耐晒艳BBC插入到类水滑石层间，制备一种光热稳定型耐晒艳红BBC插层颜料。
前面文献中报道的萘蓝黑10B和甲基橙都是一种染料，均能溶于水，而本发明中所用的耐晒艳红BBC则是一种色淀颜料，既不溶于水也不溶于大多数有机溶剂，因此要选择合适的插层反应溶剂，才能将耐晒艳红BBC插层到LDHs中。
本发明以层间阴离子为NO3 -的类水滑石为前体，采用离子交换法使耐晒艳红BBC的阴离子取代水滑石层间的NO3 -离子，生成层间阴离子为耐晒艳红BBC阴离子的插层水滑石(LDH-BBC)。
本发明制备的LDH-BBC的化学通式为：[M2+ 1-xM3+ x(OH)2](BBC)2- x/2·mH2O，其中0.2＜X/(1-X)＜0.5，m＝1-3X/2；M2+为二价金属离子Mg2+、Zn2+、Ni2+、Fe2+或Cu2+中的任意一种，M3+为三价金属离子Al3+、Fe3+或Cr3+中的任意一种。
LDH-BBC的制备步骤如下：
A.采用单滴法制备结构通式为：[M2+ 1-xM3+ x(OH)2](NO3)- x·mH2O的水滑石前体，其中0.2＜X/(1-X)＜0.5，m＝1-3X/2；将该水滑石加入高沸点的有机溶剂乙二醇、乙二醇二丁基醚或二甘醇二乙醚中，室温下磁力搅拌，配制成浓度为0.05-0.1M的水滑石悬浮液备用；
B.按照耐晒艳红BBC与水滑石前体的摩尔比为1.5-3的比例计量，将耐晒艳红BBC溶解在与步骤A相同的有机溶剂中，使其浓度控制在0.02-0.05M；
C.将步骤B制备的耐晒艳红BBC溶液与步骤A制备的水滑石悬浮液充分混合，在温度为90-150℃的条件下反应6-48h，过滤、洗涤到中性，在60-100℃干燥12-24h，得到耐晒艳红BBC阴离子插层水滑石LDH-BBC。
步骤A中所用的有机溶剂较佳的是乙二醇。
将得到的LDH-BBC进行XRD、FT-IR、UV-Vis和TG-DTA等表征显示，耐晒艳红BBC阴离子已组装进入了层状材料LDH层间。
分别按LDH-BBC、耐晒艳红BBC与PP材料的质量比为0.2％的比例，将该两种颜料复合到PP中，制成标准色板，然后用TC-P2A型全自动测色仪测定两种色板的色差(ΔE)，结果ΔE均小于5，证明插层颜料LDH-BBC保持了耐晒艳红BBC原有的颜色。把这两种复合材料同时置于功率为2000瓦的紫外灯下分别照射20、40、60和80分钟后，用测色仪测定其色差大小，结果见表1。从表1中可以看出，插层颜料LDH-BBC的耐光性明显高于耐晒艳红BBC。
表1.LDH-BBC与耐晒艳红BBC的耐光性试验结果
| 照射时间(分钟) | 20 | 40 | 60 | 80 |
| BBC(ΔE)LDH-BBS(ΔE) | 2.711.13 | 4.421.51 | 6.043.29 | 8.623.52 |
将插层颜料LDH-BBC和耐晒艳红BBC粉末分别放在温度为100、150、200、250和300℃的烘箱中受热30分钟后取出，用UV-Vis分光光度计对其耐热性进行分析可知，耐晒艳红BBC在200℃时，其UV-Vis曲线已有较大幅度的变化，而插层颜料LDH-BBC在300℃时，其UV-Vis曲线刚刚开始有所变化。这就说明插层颜料比耐晒艳红BBC具有较高的热稳定性。
显著优点：本发明所制备的插层水滑石LDH-BBC保持了耐晒艳红BBC原有的颜色，可以作为颜料使用，并且这种新型颜料的光、热稳定性与耐晒艳红BBC相比有大幅度的提高，因此用LDH-BBC代替耐晒艳红BBC用于复合材料中可大幅度减缓其退色程度和速度。所采用的前体制备方法简便，选择高沸点的有机溶剂可使耐晒艳红BBC顺利插层到水滑石中。该LDH-BBC颜料还可代替耐晒艳红BBC用于涂料和油漆中。
具体实施方式：
实施例1：
步骤A：取Mg(NO3)2·6H2O(15.38g，0.06mol)和Al(NO3)3·9H2O(11.25g，0.03mol)混合，溶于50ml脱除CO2的去离子水中；另取NaOH(7.20g，0.18mol)溶于75ml脱除CO2的去离子水中，置于250ml三口瓶中；在N2保护下将混合盐溶液缓慢滴入碱液中，强烈搅拌，然后用0.1M的NaOH溶液调节反应体系的pH值为10，接着将该浆状液于65℃的温度下陈化39h，最后抽滤、水洗得水滑石前体，其结构式为：Mg4Al2(OH)12(NO3)2·4H2O；将该水滑石前体2.20g(0.004mol)分散在50ml乙二醇中待用。
步骤B：按照耐晒艳红BBC与水滑石前体的摩尔比为1.5的比例来称取耐晒艳红BBC(2.75g，0.006mol)，使其溶于100ml乙二醇中。
步骤C：将耐晒艳红BBC溶液和LDHs前体悬浮液在容器中混合，然后在N2保护下，90℃搅拌反应48h，过滤、洗涤至pH值约为7，100℃干燥18h，组装得到耐晒艳红BBC阴离子插层LDHs材料。
分别采用XRD、FT-IR、UV-Vis和TG-DTA等手段分析和表征得到的插层LDHs，证明该插层产物层间阴离子全部为耐晒艳红BBC阴离子，是一种晶体晶相单一、结构一致的超分子插层结构材料。插层颜料与耐晒艳红BBC相比，其色差ΔE小于3，说明插层颜料与耐晒艳红BBC的颜色基本一致。通过对该插层颜料进行光、热稳定性能的测试后可知，其耐光、耐热性能均比耐晒艳红BBC有明显提高。
实施例2：
步骤A：取Mg(NO3)2·6H2O(17.31g，0.0675mol)和Al(NO3)3·9H2O(8.44g，0.0225mol)混合，溶于50ml脱除CO2的去离子水中。另取NaOH(7.20g，0.18mol)溶于75ml脱除CO2的去离子水中，置于250ml三口瓶中。在N2保护下将混合盐溶液缓慢滴入碱液中，强烈搅拌，然后用0.1M的NaOH溶液调节反应体系的pH值为10。接着将浆状液于65℃的温度下陈化39h，最后抽滤、水洗得水滑石前体，其结构式为：Mg6Al2(OH)16(NO3)2·4H2O；将该水滑石3.34g(0.005mol)分散在50ml乙二醇中。
步骤B：按照耐晒艳红BBC与水滑石前体的摩尔比为2.0的比例来称取耐晒艳红BBC(4.59g，0.01mol)，使其溶于200ml乙二醇中。
步骤C：将BBC溶液和LDHs前体悬浮液在容器中混合，然后在N2保护下，100℃搅拌反应24h，过滤、洗涤至pH值约为7，70℃干燥24h，组装得到耐晒艳红阴离子插层材料LDH-BBC。
分别采用XRD、FT-IR、UV-Vis和TG-DTA等手段分析和表征得到的插层材料，证明该插层产物层间阴离子全部为BBC阴离子，是一种晶体晶相单一、结构一致的超分子插层结构材料。插层颜料LDH-BBC与BBC相比，其色差ΔE小于5，说明该插层颜料LDH-BBC与BBC的颜色非常接近。通过对该插层颜料进行光、热稳定性能的测试后发现，其耐光、耐热性能也均比耐晒艳红BBC有明显提高。
实施例3：
步骤A：取Zn(NO3)2·6H2O(17.85g，0.06mol)、Al(NO3)3·9H2O(11.25g，0.03mol)和NaNO3(4.53g，0.053mol)混合，溶于80ml脱除CO2的去离子水中，置于250ml三口瓶中。另取NaOH(5.32g，0.133mol)溶于50ml脱除CO2的去离子水中。在N2保护下将NaOH碱溶液缓慢滴入混合盐溶液中，强烈搅拌，至pH＝6时停止滴加碱溶液。接着将浆状液于70℃的温度下陈化24h，最后抽滤、水洗得水滑石前体，其结构式为：Zn4Al2(OH)12(NO3)2·4H2O；将该水滑石2.15g(0.003mol)分散在50ml乙二醇中。
步骤B：按照耐晒艳红BBC与水滑石前体的摩尔比为1.5的比例来称取耐晒艳红BBC(2.06g，0.0045mol)，使其溶于100ml乙二醇中。
步骤C：将耐晒艳红BBC溶液和LDHs前体悬浮液在容器中混合，然后在N2保护下，95℃搅拌反应36h，过滤、洗涤至pH值约为7，70℃干燥18h，组装得到耐晒艳红BBC阴离子插层LDHs材料。
分别采用XRD、FT-IR、UV-Vis和TG-DTA等手段分析和表征得到的插层LDHs，证明该插层产物层间阴离子全部为耐晒艳红BBC阴离子，是一种晶体晶相单一、结构一致的超分子插层结构材料。插层颜料与耐晒艳红BBC相比，其色差ΔE小于5，说明插层颜料保持了耐晒艳红BBC原来的颜色。通过对该插层颜料进行光、热稳定性能的测试后可知，其耐光、耐热性能均比耐晒艳红BBC有明显提高。
Claims (4)
1.一种超分子结构光热稳定型耐晒艳红BBC颜料，其特征是该颜料是一种层间阴离子为耐晒艳红BBC阴离子的插层水滑石LDH-BBC，其化学通式为：
[M2+ 1-xM3+ x(OH)2](BBC)2- x/2·mH2O，
其中0.2＜X/(1-X)＜0.5，m＝1-3X/2；M2+为二价金属离子Mg2+、Zn2+、Ni2+、Fe2+或Cu2+中的任意一种，M3+为三价金属离子Al3+、Fe3+或Cr3+中的任意一种。
2.根据权利要求1所述的超分子结构光热稳定型耐晒艳红BBC颜料，其特征是该颜料与耐晒艳红BBC颜色的色差ΔE小于5，且其光热稳定性能比耐晒艳红BBC有大幅度提高。
3.一种超分子结构光热稳定型耐晒艳红BBC颜料的制备方法，步骤如下：
A.采用单滴法制备结构通式为：[M2+ 1-xM3+ x(OH)2](NO3)- x·mH2O的水滑石前体，其中0.2＜X/(1-X)＜0.5，m＝1-3X/2；将该水滑石加入有机溶剂乙二醇、乙二醇二丁基醚或二甘醇二乙醚中，室温下磁力搅拌，配制成浓度为0.05-0.1M的水滑石悬浮液备用；
B.按照耐晒艳红BBC与水滑石前体的摩尔比为1.5-3的比例计量，将耐晒艳红BBC溶解在与步骤A相同的有机溶剂中，使其浓度控制在0.02-0.05M；
C.将步骤B制备的耐晒艳红BBC溶液与步骤A制备的水滑石悬浮液充分混合，在温度为90-150℃的条件下反应6-48h，过滤、洗涤到中性，在60-100℃干燥12-24h，得到耐晒艳红BBC阴离子插层水滑石LDH-BBC。
4.根据权利要求3所述的超分子结构光热稳定型耐晒艳红BBC颜料的制备方法，其特征是步骤A中所述的有机溶剂是乙二醇。
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| PCT/CN2004/001116 WO2005047397A1 (fr) | 2003-11-13 | 2004-09-28 | Pigment bbc rouge permanent a structure supramoleculaire constituant un moyen de stabilisation de lumiere et de chaleur et son procede de preparation |
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| CN1294213C (zh) * | 2004-06-24 | 2007-01-10 | 北京化工大学 | 一种光热稳定型甲基橙插层颜料及其应用 |
| CN1333005C (zh) * | 2005-12-19 | 2007-08-22 | 北京化工大学 | 超分子插层结构紫外光吸收剂及其制备方法和用途 |
| CN101879314B (zh) * | 2009-12-08 | 2012-05-30 | 山东炳坤腾泰陶瓷科技有限公司 | 一种生物药物/类水滑石复合材料的合成方法 |
| CN101982509A (zh) * | 2010-10-08 | 2011-03-02 | 北京化工大学 | 一种光、热稳定型超分子结构酸性黄17插层颜料及其制备方法 |
| CN102732055A (zh) * | 2011-04-07 | 2012-10-17 | 北京化工大学 | 多组分显色阴离子共插层超分子结构颜料及其制备方法 |
| CN103965654B (zh) * | 2014-04-30 | 2016-08-17 | 北京化工大学 | 一种耐光型超分子插层结构颜料及其制备方法 |
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| CN1056827A (zh) * | 1990-05-25 | 1991-12-11 | 密歇根州州立大学托管委员会 | 多酸根嵌入的层状复氢氧化物 |
| US5414080A (en) * | 1992-11-25 | 1995-05-09 | Board Of Trustees Operating Michigan State University | Porphyrin-metallic complex intercalated layered double hydroxides |
| CN1171979A (zh) * | 1996-07-29 | 1998-02-04 | 德国泰克萨科股份公司 | 制备水滑石及其金属氧化物的方法 |
| US5730951A (en) * | 1994-04-29 | 1998-03-24 | Aluminum Company Of America | Two powder synthesis of hydrotalcite and hydrotalcite-like compounds with polyvalent inorganic anions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1056827A (zh) * | 1990-05-25 | 1991-12-11 | 密歇根州州立大学托管委员会 | 多酸根嵌入的层状复氢氧化物 |
| US5414080A (en) * | 1992-11-25 | 1995-05-09 | Board Of Trustees Operating Michigan State University | Porphyrin-metallic complex intercalated layered double hydroxides |
| US5730951A (en) * | 1994-04-29 | 1998-03-24 | Aluminum Company Of America | Two powder synthesis of hydrotalcite and hydrotalcite-like compounds with polyvalent inorganic anions |
| CN1171979A (zh) * | 1996-07-29 | 1998-02-04 | 德国泰克萨科股份公司 | 制备水滑石及其金属氧化物的方法 |
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