CN115626975B - 一种防沉剂以及相应的防沉降颜料糊的制备方法 - Google Patents
一种防沉剂以及相应的防沉降颜料糊的制备方法 Download PDFInfo
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Abstract
本发明涉及一种新型防沉剂以及相应的防沉降颜料糊的制备方法，包括以下步骤：向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入二元醇、饱和二元酸或酸酐，升温至200～230℃进行缩聚脱水反应，反应至酸值4.0～10.0mgKOH/g且Gardner泡管粘度大于U，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合；反应产物降温加入阻聚剂后得到防沉剂；再将20～80质量份的无稀释剂不饱和聚酯树脂、80～20质量份的无机颜料粉、0.4～4.0质量份的防沉剂，在高速剪切分散机中搅拌均匀并研磨后得到防沉降颜料糊。本发明的防沉剂防沉降性好，加入颜料糊中，会明显改善颜料糊的沉降情况，使颜料糊在长期放置时不易沉降。
Description
技术领域
本发明涉及一种新型防沉剂以及相应的防沉降颜料糊的制备方法，属于有机高分子化合物制备技术领域。
背景技术
颜料糊是由基体树脂与各色颜料粉经混合、研磨而成，具有色泽均匀、亮度高、固化无变色、色差小等优点。颜料糊具备良好的着色性，与颜料粉相比，颜料糊使用方便。
在颜料糊生产过程中，无机颜料粉在外力的作用下，成为细小的颗粒，均匀地分布到连续相中，得到一个悬浮体。颜料糊在贮存过程中，其固体组分会出现下沉甚至至容器底部的现象，称为沉降。这是由于颜料粉分散完成后，当体系中的剪切应力一旦减弱或消失时，由于颜料粉颗粒研磨不均、分散不良、以及颜料粉密度大等因素，分散在介质中的颜料细颗粒就有可能再次凝聚，又回到团聚体的状态，在重力的作用下导致颜料糊在贮存期间沉降。在沉降现象严重时，容器底部出现结块，不易再分散，会严重影响颜料糊的后期使用。为减少沉降问题，一般会在配置颜料糊时加入少量触变助剂，如气相二氧化硅和有机膨润土，它们会提高颜料糊的触变，延长防沉降时间，但气相二氧化硅和有机膨润土本身在长期放置时也会沉降，而且在使用时会受到环境等因素的影响，失去触变性效果，导致颜料糊出现沉降问题。
发明内容
本发明要解决的技术问题是提供一种防沉降性好的新型防沉剂，采用该防沉剂制备的颜料糊，会明显改善颜料糊的沉降情况，使颜料糊在长期放置时不易沉降，从而延长颜料糊的储存时间。
本发明为解决上述技术问题提供的一种技术方案是：一种新型防沉剂的制备方法，包括以下步骤：向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入反应物，所述反应物包括二元醇和饱和二元酸，升温至200～230℃进行缩聚脱水反应，反应至酸值4.0～10.0mgKOH/g且Gardner泡管粘度大于U，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合；反应产物降温加入阻聚剂后得到防沉剂；所述饱和二元酸是丁二酸、戊二酸、己二酸、庚二酸中的一种或多种。反应产物的重均分子量大于4000。
上述反应物还可以包括苯环类饱和二元酸，所述苯环类饱和二元酸是邻苯二甲酸酐、间苯二甲酸、对苯二甲酸中的一种或多种。
上述二元醇是乙二醇、丙二醇、一缩二乙二醇、一缩二丙二醇、新戊二醇、甲基丙二醇中的一种或多种；所述阻聚剂是对苯二酚、对苯醌和叔丁基邻苯二酚中的一种或多种。
本发明为解决上述技术问题提供的另一种技术方案是：一种防沉降颜料糊的制备方法，包括以下步骤：
A．向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入反应物，所述反应物包括二元醇和饱和二元酸，升温至200～230℃进行缩聚脱水反应，反应至酸值4.0～10.0mgKOH/g且Gardner泡管粘度大于U(固体/苯乙烯=2/1)；反应产物降温加入阻聚剂后得到防沉剂；所述饱和二元酸是丁二酸、戊二酸、己二酸、庚二酸中的一种或多种。反应产物的重均分子量大于4000。
B．将20～80质量份的无稀释剂不饱和聚酯树脂、80～20质量份的无机颜料粉、0.4～4.0质量份的防沉剂，在高速剪切分散机中搅拌均匀并研磨后得到防沉降颜料糊。
上述二元醇是乙二醇、丙二醇、一缩二乙二醇、一缩二丙二醇、新戊二醇、甲基丙二醇中的一种或多种。
上述反应物还可以包括苯环类饱和二元酸，所述苯环类饱和二元酸是邻苯二甲酸酐、间苯二甲酸、对苯二甲酸中的一种或多种。
上述阻聚剂是对苯二酚、对苯醌和叔丁基邻苯二酚中的一种或多种。
上述无机颜料粉是钛白粉、氧化铁棕、氧化铁红、铬黄中的一种或多种。
本发明为解决上述技术问题提供的另一种技术方案是：一种采用上述的制备方法制得的防沉降颜料糊。
本发明具有积极的效果：本发明的防沉剂由二元醇、饱和二元酸经缩聚脱水反应而成，还可以添加苯环类饱和二元酸作为反应物。通过选用碳链长度在四个或四个以上的饱和二元酸，并且控制反应的终点，使得防沉剂的分子量较大，重均分子量在4000以上，该新型防沉剂能够吸附在颜料粉的表面使颜料粉的分散体处于稳定状态，不易聚集形成大颗粒从而导致沉降。而且该新型防沉剂与无稀释剂不饱和聚酯树脂还能形成网络结构，进一步减少沉降。本发明的防沉剂防沉降性好，与气相二氧化硅和有机膨润土相比，该防沉剂与颜料糊使用的基体树脂相容性好，而且防沉降颜料糊的触变性能更好，不会出现防沉剂本身的沉降现象，在长期放置时更不容易沉降。本发明的防沉剂在使用时与不含稀释剂的不饱和聚酯树脂和无机颜料粉混合分散即可，使用方便。
具体实施方式
实施例1
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入2.0mol乙二醇、4.0mol丙二醇、3.0mol邻苯二甲酸酐、3.0mol己二酸，升温至220℃进行缩聚脱水反应，反应至酸值6.0mgKOH/g，Gardner泡管粘度U，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的对苯二酚，得到防沉剂。
B．将称重好的50质量份的无稀释剂不饱和聚酯树脂HRM6100，0.6质量份的防沉剂，50质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
实施例2
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入1.5mol乙二醇、3.5mol甲基丙二醇、2.0mol间苯二甲酸、3.0mol戊二酸，升温至225℃进行缩聚脱水反应，反应至酸值4.0mgKOH/g，Gardner泡管粘度V，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的对苯醌，得到防沉剂。
B．将称重好的70质量份的无稀释剂不饱和聚酯树脂HRM6100，0.4质量份的防沉剂，30质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
实施例3
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入2.0mol丙二醇、3.0mol一缩二丙二醇、2.0mol对苯二甲酸、3.0mol己二酸，升温至225℃进行缩聚脱水反应，反应至酸值10.0mgKOH/g，Gardner泡管粘度W，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的叔丁基邻苯二酚，得到防沉剂。
B．将称重好的30质量份的无稀释剂不饱和聚酯树脂HRM6100，1.0质量份的防沉剂，70质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
实施例4
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入1.0mol丙二醇、2.0mol一缩二丙二醇、3.0mol戊二酸，升温至230℃进行缩聚脱水反应，反应至酸值8.0mgKOH/g，Gardner泡管粘度W，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的对苯二酚，得到防沉剂。
B．将称重好的50质量份的无稀释剂不饱和聚酯树脂HRM6100，1.0质量份的防沉剂，50质量份的氧化铁红，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
实施例5
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入2.0mol丙二醇、3.0mol一缩二丙二醇、2.0mol对苯二甲酸、3.0mol己二酸，升温至225℃进行缩聚脱水反应，反应至酸值6.0mgKOH/g，Gardner泡管粘度W，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的对苯二酚，得到防沉剂。
B．将称重好的50质量份的无稀释剂不饱和聚酯树脂HRM6100，0.6质量份的防沉剂，50质量份的铬黄，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
实施例6
本实施例的防沉降颜料糊的制备方法的具体步骤如下：
A. 向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入1.0mol乙二醇、1.0mol丙二醇、1.0mol丁二酸、1.0mol己二酸，升温至230℃进行缩聚脱水反应，反应至酸值6.0mgKOH/g，Gardner泡管粘度X，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合，降温至150℃，加入反应产物总质量200ppm的对苯二酚，得到防沉剂。
B．将称重好的50质量份的无稀释剂不饱和聚酯HRM6210，0.6质量份的防沉剂，50质量份的氧化铁红，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
对比例1
本对比例的防沉降颜料糊的制备方法的具体步骤如下：
将称重好的50质量份的无稀释剂不饱和聚酯HRM6100，50质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
对比例2
本对比例的防沉降颜料糊的制备方法的具体步骤如下：
将称重好的50质量份的无稀释剂不饱和聚酯HRM6100，0.6质量份的有机膨润土，50质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
对比例3
本对比例的防沉降颜料糊的制备方法的具体步骤如下：
将称重好的50质量份的无稀释剂不饱和聚酯HRM6100，0.6质量份的气相二氧化硅，50质量份的钛白粉，在高速剪切分散机中搅拌均匀，研磨至细度为40μm以下得到颜料糊。
对实施例1至6的颜料糊和对比例1至3的颜料糊进行检测，细度检测标准是ASTMD1210，粘度和触变的检测标准是JIS K 6901液体不饱和聚酯树脂试验方法，检测结果如表1所示。
表1 不同配比颜料糊的性能对比表
本发明新型防沉剂粘度较大，与无机颜料和不含稀释剂（苯乙烯等）的不饱和聚酯树脂混合制成颜料糊后，粘度大，触变性能好，六个月颜料糊不会发生颜料沉降，防沉降效果优于有机膨润土和气相二氧化硅。
显然，上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而这些属于本发明的精神所引伸出的显而易见的变化或变动仍处于本发明的保护范围之中。
Claims (6)
1.一种防沉降颜料糊的制备方法，其特征在于，包括以下步骤：
A．向装有氮气保护、搅拌器、温度计和冷凝分馏装置的四口容器中加入反应物，所述反应物包括二元醇和饱和二元酸，升温至200～230℃进行缩聚脱水反应，反应至酸值4.0～10.0mgKOH/g且Gardner泡管粘度大于U，测定泡管粘度是将反应产物与苯乙烯按照质量比为2:1进行混合；反应产物降温加入阻聚剂后得到防沉剂；所述饱和二元酸是丁二酸、戊二酸、己二酸、庚二酸中的一种或多种；
B．将20～80质量份的无稀释剂不饱和聚酯树脂、80～20质量份的无机颜料粉、0.4～4.0质量份的步骤A得到的防沉剂，在高速剪切分散机中搅拌均匀并研磨后得到防沉降颜料糊。
2.根据权利要求1所述的防沉降颜料糊的制备方法，其特征在于：所述二元醇是乙二醇、丙二醇、一缩二乙二醇、一缩二丙二醇、新戊二醇、甲基丙二醇中的一种或多种。
3.根据权利要求2所述的防沉降颜料糊的制备方法，其特征在于：所述反应物还包括邻苯二甲酸酐、间苯二甲酸、对苯二甲酸中的一种或多种。
4.根据权利要求2所述的防沉降颜料糊的制备方法，其特征在于：所述阻聚剂是对苯二酚、对苯醌和叔丁基邻苯二酚中的一种或多种。
5.根据权利要求2所述的防沉降颜料糊的制备方法，其特征在于：所述无机颜料粉是钛白粉、氧化铁棕、氧化铁红、铬黄中的一种或多种。
6.一种采用如权利要求1所述的制备方法制得的防沉降颜料糊。
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