CN107445904A - 嘧啶‑十八烷基季铵盐荧光增白剂及其制备方法和应用 - Google Patents
嘧啶‑十八烷基季铵盐荧光增白剂及其制备方法和应用 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- -1 Pyrimidine octadecyl quaternary ammonium salt Chemical class 0.000 title claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 19
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- 239000007864 aqueous solution Substances 0.000 claims description 22
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- 238000006243 chemical reaction Methods 0.000 claims description 13
- BTTNYQZNBZNDOR-UHFFFAOYSA-N 2,4-dichloropyrimidine Chemical compound ClC1=CC=NC(Cl)=N1 BTTNYQZNBZNDOR-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- TYWAOIBYSDORAH-UHFFFAOYSA-N 1,2-bis(4-aminophenyl)ethane-1,2-dione Chemical compound C1=CC(N)=CC=C1C(=O)C(=O)C1=CC=C(N)C=C1 TYWAOIBYSDORAH-UHFFFAOYSA-N 0.000 claims description 7
- 238000005282 brightening Methods 0.000 claims description 6
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- 229910052708 sodium Inorganic materials 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 4
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- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
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- 229910001424 calcium ion Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
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- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/20—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D239/22—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with hetero atoms directly attached to ring carbon atoms
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Abstract
本发明提供一种嘧啶‑十八烷基季铵盐荧光增白剂，其特征在于，所述的嘧啶‑十八烷基季铵盐荧光增白剂的结构式如式1所示：本发明的目的在于提供一种嘧啶‑十八烷基季铵盐荧光增白剂及其制备方法和应用，该制备方法简单，原材料价格低廉。采用本发明嘧啶‑十八烷基季铵盐荧光增白剂处理重质碳酸钙粉体具有较高的白度和亮度，是一种高性能重质碳酸钙粉体荧光增白剂。
Description
技术领域
本发明涉及荧光增白剂技术领域，具体涉及一种嘧啶-十八烷基季铵盐荧光增白剂及其制备方法和应用。
背景技术
我国在“十二五”新材料发展规划中将开发与资源、环境协调的新材料作为主要考核指标，通过开发新材料解决资源短缺问题。我国已经形成了比较完善的材料科技体系，在某些新材料领域内具有明显的资源优势和技术优势，但总体自主创新能力还比较薄弱，具有自主知识产权的新材料产品及技术还比较少，尤其是在重质碳酸钙粉体荧光增白材料方面创新性不足。
荧光增白剂具有很高的光量子产率，对被处理的基质能有效地增白、増艳。荧光增白剂分子具有较大的共轭体系，能够吸收波长范围在300～400nm左右的紫外光，并发射出波长范围在420～450nm左右的蓝色荧光，从而弥补了基质中由于蓝光缺失而造成的视觉上的泛黄。通过弥补蓝光使人感到被处理的基质更亮洁、更鲜艳。荧光增白剂被广泛地用于造纸、纺织、洗涤剂、塑料、油墨、皮革、紫外吸收剂、显影剂等诸多领域，市场需求巨大。
重质碳酸钙作为最大的无机填料，由于原料广、价格低、无毒等优点，被广泛应用于电缆料、合成革、聚乙烯薄膜，泡沫塑料、塑料管材、纸张等制品的填充料或原料。重质碳酸钙粉体作为最大填充材料，人们对其白度和亮度均有较高要求，市场上有众多塑料、造纸和洗涤剂等专用荧光增白剂，但重质碳酸钙粉体荧光增白剂却很少见，市场需求非常迫切和巨大。
重质碳酸粉体表面具有游离钙离子和羟基，市场上现有的荧光增白剂很难与重质碳酸钙粉体表面离子键合或表面吸附，因此缺乏能有效增白、增亮重质碳酸钙粉体的荧光增白剂。
发明内容
针对上述不足，本发明的目的在于提供一种嘧啶-十八烷基季铵盐荧光增白剂及其制备方法和应用，该嘧啶-十八烷基季铵盐荧光增白剂合成方法简单，原料价格低廉。通过测试嘧啶-十八烷基季铵盐荧光增白剂的光学性能，可以明显看出嘧啶-十八烷基季铵盐荧光增白剂具有较强的紫外吸收性能。嘧啶-十八烷基季铵盐荧光增白剂对重质碳酸钙粉体具有较强的键合力和显著的增白、增亮作用。嘧啶-十八烷基季铵盐荧光增白剂是一种新型高性能重质碳酸钙粉体荧光增白剂，具有极大的推广和应用空间。
具体来说，本发明的方案为：一种嘧啶-十八烷基季铵盐荧光增白剂，所述的嘧啶-十八烷基季铵盐荧光增白剂的结构式如式1：
同时本发明还公开了上述一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，包括以下步骤：
步骤1：将4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液加入到2,4-二氯嘧啶溶液中，用 10％Na2CO3水溶液维持体系的pH值为7～8，在20～25℃搅拌反应一段时间；
步骤2：然后将二甲十八烷基叔胺加入到步骤1的反应混合物中，用10％Na2CO3水溶液维持体系的pH值为8～9，回流反应一段时间；
步骤3：冷却反应混合物至室温，加入无机盐，使嘧啶-十八烷基季铵盐荧光增白剂析出并收集；
其中，4,4'-二氨基二苯乙烯-2,2'-二磺酸、2,4-二氯嘧啶、二甲十八烷基叔胺物质量的比例为：1:2.1:1.95。
在上述一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，所述的步骤1中，2,4-二氯嘧啶溶液中，每10mmol 2,4-二氯嘧啶对应10～15mL二甲基甲酰胺；4,4'-二氨基二苯乙烯-2,2'- 二磺酸水溶液中，每5mmol 4,4'-二氨基二苯乙烯-2,2'-二磺酸对应50～55mL水。
在上述嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，所述的4,4'-二氨基二苯乙烯-2,2'- 二磺酸水溶液的pH值为5～6。
在上述嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，pH值用10％Na2CO3水溶液调控。
在上述的嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，所述的步骤1的反应时间为10～11小时；所述的步骤2的反应时间为6～7小时。
在上述嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，步骤3中的无机盐为氯化钠。
在上述嘧啶-十八烷基季铵盐荧光增白剂的制备方法中，所述的步骤1中，4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液以滴加的形式加入到2,4-二氯嘧啶溶液中。
另外本发明还提供了一种嘧啶-十八烷基季铵盐荧光增白剂的用途，用于重质碳酸钙粉体的增白和增亮。
本发明与传统方法相比，具有以下优势：
1.本发明嘧啶-十八烷基季铵盐荧光增白剂合成方法简单，原材料价格低廉。
2.本发明嘧啶-十八烷基季铵盐荧光增白剂能与重质碳酸钙粉体表面离子发生有效化学键合，结合牢固度高，耐候性更好；
3.本发明嘧啶-十八烷基季铵盐荧光增白剂具有较强的紫外吸收性能，可以显著地增白、增亮重质碳酸钙粉体，是一种新型高性能荧光增白剂。
附图说明
图1为实施例3的嘧啶-十八烷基季铵盐荧光增白剂水溶液的光学性能测试中紫外吸收谱图。
具体实施例
下面结合具体实施方式对本发明的权利要求做进一步的详细说明，但不构成对本发明的任何限制，任何在本发明权利要求范围内所做的有限修改，仍在本发明的权利要求保护范围内。
实施例1
21mmol 2,4-二氯嘧啶加到22mL二甲基甲酰胺中，25℃搅拌。而后滴加10mmol 4,4'- 二氨基二苯乙烯-2,2'-二磺酸与100mL蒸馏水的混合液，用10％Na2CO3水溶液维持反应体系的pH＝7，25℃反应11h。而后加19.5mmol二甲基十八叔胺，用10％Na2CO3水溶液维持体系的pH＝9，回流反应7h。用薄层色谱技术监测两步反应终点。冷却至室温，加入20g氯化钠，搅拌、抽滤，真空干燥得嘧啶-十八烷基季铵盐荧光增白剂，收率87％。
实施例2
21mmol 2,4-二氯嘧啶加到31.5mL二甲基甲酰胺中，20℃搅拌。而后滴加10mmol4,4'- 二氨基二苯乙烯-2,2'-二磺酸与110mL蒸馏水的混合液，用10％Na2CO3水溶液维持反应体系的pH＝8，25℃反应10h。而后加19.5mmol二甲基十八叔胺，用10％Na2CO3水溶液维持体系的pH＝8，回流反应6h。用薄层色谱技术监测两步反应终点。冷却至室温，加入20g氯化钠，搅拌、抽滤，真空干燥得嘧啶-十八烷基季铵盐荧光增白剂，收率83％。
实施例3
21mmol 2,4-二氯嘧啶加到26mL二甲基甲酰胺中，25℃搅拌。而后滴加10mmol 4,4'- 二氨基二苯乙烯-2,2'-二磺酸与100mL蒸馏水的混合液，用10％Na2CO3水溶液维持反应体系的pH＝7.5，25℃反应11h。而后加19.5mmol二甲基十八叔胺，用10％Na2CO3水溶液维持体系的pH＝9，回流反应7h。用薄层色谱技术监测两步反应终点。冷却至室温，加入20g氯化钠，搅拌、抽滤，真空干燥得嘧啶-十八烷基季铵盐荧光增白剂，收率84.5％。
光学性能测试
本发明采用紫外-可见光谱对本发明产物进行光学性能测试，紫外吸收谱图如图1所示。
紫外-可见光谱可以有效地测试荧光增白剂分子的共轭体系。嘧啶-十八烷基季铵盐荧光增白剂配制成浓度为0.02g/L的水溶液进行光学性能测试。测试结果表明，嘧啶-十八烷基季铵盐荧光增白剂有较强的紫外吸收性能，最大吸收峰位于348nm。
增白性能测试
配制嘧啶-十八烷基季铵盐荧光增白剂质量浓度为0.01～0.03％的水溶液100mL，处理100 g不同粒度和白度的重质碳酸钙粉体。具体做法如下：将不同粒径和白度的重质碳酸钙粉体放入适量上述浓度的溶液中，室温搅拌30min，抽干，干燥，即可得到高白、高亮重质碳酸钙粉体。
实验结果证明，该嘧啶-十八烷基季铵盐荧光增白剂对不同品质的碳酸钙粉体有显著的增白、增亮效果，在浓度为0.02％时，处理粒度为400～2500目，白度为91～95的重质碳酸钙粉体，其白度增加值介于1～2.5之间。嘧啶-十八烷基季铵盐荧光增白剂是一种新型高性能重质碳酸钙粉体荧光增白，具有极大的推广和应用空间。
以上所述的仅为本发明的较佳实施例，凡在本发明的精神和原则范围内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围内。
Claims (9)
1.一种嘧啶-十八烷基季铵盐荧光增白剂，其特征在于，所述的一种嘧啶-十八烷基季铵盐荧光增白剂的结构式如式1：
2.一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，包括以下步骤：
步骤1：将4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液加入到2,4-二氯嘧啶溶液中，用10％Na2CO3水溶液维持体系的pH值为7～8，在20～25℃搅拌反应一段时间；
步骤2：然后将二甲基十八烷基叔胺加入到步骤1的反应混合物中，用10％Na2CO3水溶液维持体系的pH值为8～9，回流反应一段时间；
步骤3：冷却反应混合物至室温，加入无机盐，使嘧啶-十八烷基季铵盐荧光增白剂析出并收集；
其中，4,4'-二氨基二苯乙烯-2,2'-二磺酸、2,4-二氯嘧啶和二甲基十八烷基叔胺物质量的比例为：1:2.1:1.95。
3.根据权利要求2所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，所述的步骤1中，2,4-二氯嘧啶溶液中，每10mmol 2,4-二氯嘧啶对应10～15mL二甲基甲酰胺；4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液中，每5mmol 4,4'-二氨基二苯乙烯-2,2'-二磺酸对应50～55mL水。
4.根据权利要求2所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，所述的4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液的pH值为5～6。
5.根据权利要求2或4所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，pH值用10％Na2CO3水溶液调控。
6.根据权利要求2所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，所述步骤1的反应时间为10～11小时；所述的步骤2的反应时间为6～7小时。
7.根据权利要求2所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，步骤3中的无机盐为氯化钠。
8.根据权利要求2所述的一种嘧啶-十八烷基季铵盐荧光增白剂的制备方法，其特征在于，所述的步骤1中，4,4'-二氨基二苯乙烯-2,2'-二磺酸水溶液以滴加的形式加入到2,4-二氯嘧啶溶液中。
9.权利要求1所述的一种嘧啶-十八烷基季铵盐荧光增白剂的用途，其特征在于，用于重质碳酸钙粉体的增白、增亮。
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| CN102504570A (zh) * | 2011-09-26 | 2012-06-20 | 山东大学 | 含双醚类季铵盐型荧光增白剂及其合成和应用 |
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| CN102504570A (zh) * | 2011-09-26 | 2012-06-20 | 山东大学 | 含双醚类季铵盐型荧光增白剂及其合成和应用 |
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