CN108410319B - 珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法 - Google Patents

珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法 Download PDF

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CN108410319B
CN108410319B CN201810246653.6A CN201810246653A CN108410319B CN 108410319 B CN108410319 B CN 108410319B CN 201810246653 A CN201810246653 A CN 201810246653A CN 108410319 B CN108410319 B CN 108410319B
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伍家卫
吕维华
张海亮
马庭洲
索陇宁
张歆婕
尚秀丽
周锦
张�浩
周艳青
田华
唐蓉萍
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Lanzhou Petrochemical College of Vocational Technology
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Abstract

本发明公开了一种珍珠岩‑氰尿酸三聚氰胺固化制备超支化环氧底漆的方法，是将环氧树脂、轻质碳酸钙、氧化铁红、滑石粉、锌黄溶解于混合溶剂得组分
Figure 100004_DEST_PATH_IMAGE002
；将珍珠岩‑氰尿酸三聚氰胺固化剂溶解于二甲苯中，得组分
Figure 518658DEST_PATH_IMAGE002
Figure 435798DEST_PATH_IMAGE002
；然后将组分
Figure 746694DEST_PATH_IMAGE002
、组分

Description

珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法
技术领域
本发明涉及一种超支化环氧底漆的制备，尤其涉及一种以珍珠岩-氰尿酸三聚氰胺为复合固化剂制备超支化环氧底漆的方法，属于涂料化工技术领域。
背景技术
超支化环氧树脂是一种具有低粘度、高环氧值、高活性、低voc的高分子量环氧树脂，可作为环氧树脂、环硫树脂等热固性树脂的稀释剂、增强增韧助剂；也可作为牙科修复材料、灌封涂料、电子封装涂料增强增韧助剂、消泡剂；也可作为合成其他功能高分子材料的中间体，应用于航空航天等高端领域的涂 料、热固性塑料、胶黏剂等。在超支化环氧环氧树脂的制备中，环氧固化剂起着决定性的作用，环氧固化剂的选择会直接影响超支化环氧树脂的固化速度，交联密度，从而影响超支化环氧树脂的各项性能。
发明内容
本发明的目的是提供一种以珍珠岩-氰尿酸三聚氰胺为复合固化剂制备超支化环氧底漆的方法。
一、本发明双组份超支化环氧底漆的制备
（1）环氧固化剂的制备：先将氰尿酸三聚氰胺溶解于由乙醇、正丁醇、醋酸丁酯组成的混合溶剂（乙醇、正丁醇、醋酸丁酯的体积比为1:1:1~5:5:1）中，配成浓度为0.1~1g/ml的混合液；再将珍珠岩和膨润土按0.5~5g/ml的固液比添加到上述混合液中，在30~50℃下搅拌5~6小时，研磨至80µm以下即得；
（2）组分
Figure 947735DEST_PATH_IMAGE001
的制备：将环氧树脂、轻质碳酸钙、氧化铁红、滑石粉、锌黄溶解于混合溶剂得组分
Figure 832252DEST_PATH_IMAGE001
；且各组分按以下重量份配比：环氧树脂20~30份，轻质碳酸钙20~30份，氧化铁红10~15份，滑石粉10~20份，锌黄5~10份，混合溶剂40~60份；其中混合溶剂由甲苯、丙酮、醋酸乙酯、醋酸丁酯按4:1:1:1~5:2:2.5:1的质量比混合而成；
（3）组分
Figure 100002_DEST_PATH_IMAGE002
的制备：将环氧固化剂溶解于二甲苯中，得组分
Figure 346410DEST_PATH_IMAGE001
Figure 210461DEST_PATH_IMAGE001
；环氧固化剂与二甲苯按以下重量份配比：70~80份，20~30份；
（4）双组份超支化环氧底漆的制备：将组分
Figure 228095DEST_PATH_IMAGE001
、组分
Figure 316137DEST_PATH_IMAGE002
按10:2~10:5的重量比充分混合，即得双组份超支化环氧底漆。
二、双组份超支化环氧底漆的性能
将上述制备的双组份超支化环氧底漆涂刷在贴板上，实干后进行全项性能检测，结果见表1。
Figure 52012DEST_PATH_IMAGE003
综上所述，固化剂中含氰尿酸三聚氰胺是碱性环氧树脂固化剂，而且通过一定的方式负载于珍珠岩与膨润土形成复合物。胺的固化机理为亲核加成，每一个活泼氢可以打开一个环氧基团，使之交联固化。在固化体系中含给质子基团的化合物氰尿酸三聚氰胺，更加促进胺类固化。这是一个双分子反应机理，即给质子体氰尿酸上的氢首先与环氧基上的氧形成氢键，使环氧基进一步极化，有利于三聚氰胺上的N对环氧基的亲核进攻，同时完成氢原子的加成，促进三聚氰胺固化，同时氰尿酸自身也会发生酸固化交联，所以氰尿酸三聚氰胺较纯粹的三聚氰胺固化速度更快，交联密度更大。膨润土具有高温稳定性和防沉、增稠、触变、助成膜作用。珍珠岩为多孔矿物，但因无粘性，单独使用容易沉淀，所以须与粘性膨润土复配，相辅相成。在有机溶剂作用下，晶层间距加大，因孔道效应和吸附效应，用于制备胺固化的环氧底漆，提高了涂层交联密度，从而提高了耐磨性、耐水性、抗冲击性等各项性能。固化反应方程式如下：
Figure 100002_DEST_PATH_IMAGE004
具体实施方式
下面通过具体实施例对本发明双组份超支化环氧底漆的制备和性能做进一步说明。
实施例一
（1）复合固化剂的制备：取6g 氰尿酸三聚氰胺，加入到20mL由乙醇、正丁醇、醋酸丁酯配成的混合溶剂（乙醇、正丁醇、醋酸丁酯分别为8mL、7mL、5 mL）中，配成混合液；
称取20g珍珠岩、10g膨润土，添加到上述混合液中，在35℃下搅拌5~6小时，研磨至80µm以下即得；
（2）组分
Figure 719754DEST_PATH_IMAGE001
的制备：取环氧树脂20g、轻质碳酸钙20g、氧化铁红10g、滑石粉10g、锌黄5g，溶解于40g混合溶剂，研磨至80µm以下，即得组分
Figure 591895DEST_PATH_IMAGE001
；
其中混合溶剂由甲苯、丙酮、醋酸乙酯、醋酸丁酯按4:1:1.5:1的质量比混合而成；
（3）组分
Figure 850838DEST_PATH_IMAGE002
的制备：将80g环氧固化剂溶解于20g二甲苯中，得组分
Figure 808430DEST_PATH_IMAGE001
Figure 811021DEST_PATH_IMAGE001
；
（4）双组份超支化环氧底漆的制备：将组分
Figure 27414DEST_PATH_IMAGE001
、组分
Figure 926100DEST_PATH_IMAGE002
按10:3的重量比充分混合，即得双组份超支化环氧底漆。该超支化环氧底漆的性能指标见表1。
实施例二
（1）复合固化剂的制备：取7g氰尿酸三聚氰胺，加入到20mL由乙醇、正丁醇、醋酸丁酯配成的混合溶剂（乙醇、正丁醇、醋酸丁酯分别为8mL、6mL、6 mL）中，配成混合液；
称取20g珍珠岩、10g膨润土，添加到上述混合液中，在40℃下搅拌5~6小时，研磨至80µm以下即得；
（2）组分
Figure 433305DEST_PATH_IMAGE001
的制备：取环氧树脂25g、轻质碳酸钙25g、氧化铁红12g、滑石粉15g、锌黄8g，溶解于50g混合溶剂，研磨至80µm以下即得；
其中混合溶剂由甲苯、丙酮、醋酸乙酯、醋酸丁酯按5:2:2.5:1的质量比混合而成；
（3）组分
Figure 911691DEST_PATH_IMAGE002
的制备：将70g复合固化剂溶解于30g二甲苯中，得组分
Figure 820741DEST_PATH_IMAGE001
Figure 624749DEST_PATH_IMAGE001
；
（4）双组份超支化环氧底漆的制备：将组分
Figure 353670DEST_PATH_IMAGE001
、组分
Figure 275228DEST_PATH_IMAGE002
按10:2的重量比充分混合，即得双组份超支化环氧底漆。该超支化环氧底漆的性能指标见表1。
实施例三
（1）复合固化剂的制备：取10g 氰尿酸三聚氰胺，加入到20mL 由乙醇、正丁醇、醋酸丁酯配成的混合溶剂（乙醇、正丁醇、醋酸丁酯分别为10mL、3mL、7mL）中，配成混合液；
称取15g珍珠岩、15g膨润土，添加到上述混合液中，在30℃下搅拌5~6小时，研磨至80µm以下即得；
（2）组分
Figure 382992DEST_PATH_IMAGE001
的制备：取环氧树脂30g、轻质碳酸钙30g、氧化铁红15g、滑石粉20g、锌黄10g，溶解于60g混合溶剂，研磨至80µm以下即得；
其中混合溶剂由甲苯、丙酮、醋酸乙酯、醋酸丁酯按4:1:1:1的质量比混合而成；
（3）组分
Figure 92322DEST_PATH_IMAGE002
的制备：将75g环氧固化剂溶解于25g二甲苯中，得组分
Figure 511802DEST_PATH_IMAGE001
Figure 754827DEST_PATH_IMAGE001
；
（4）双组份超支化环氧底漆的制备：将组分
Figure 513836DEST_PATH_IMAGE001
、组分
Figure 629953DEST_PATH_IMAGE002
按10:5的重量比充分混合，即得双组份超支化环氧底漆。该超支化环氧底漆的性能指标见表1。

Claims (4)

1.一种珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法，包括以下工艺步骤：
（1）环氧固化剂的制备：先将氰尿酸三聚氰胺溶解于由乙醇、正丁醇、醋酸丁酯组成的混合溶剂中，配成浓度为0.1~1g/mL的混合液；再将珍珠岩和膨润土按0.5~5g/mL的固液比添加到上述混合液中，在30~50℃下搅拌5~6小时，研磨至80µm以下即得；
（2）组分
Figure DEST_PATH_IMAGE002
的制备：是将环氧树脂、轻质碳酸钙、氧化铁红、滑石粉、锌黄溶解于混合溶剂得组分
Figure 260342DEST_PATH_IMAGE002
；且各组分按以下重量份配比：环氧树脂20~30份、轻质碳酸钙20~30份、氧化铁红10~15份、滑石粉10~20份、锌黄5~10份、混合溶剂40~60份；
（3）组分
Figure DEST_PATH_IMAGE004
的制备：将环氧固化剂溶解于二甲苯中，得组分
Figure 85472DEST_PATH_IMAGE002
Figure 865209DEST_PATH_IMAGE002
；且环氧固化剂与二甲苯的重量份为：环氧固化剂70~80份、二甲苯20~30份；
（4）双组份超支化环氧底漆的制备：将组分
Figure 260418DEST_PATH_IMAGE002
、组分
Figure 340370DEST_PATH_IMAGE004
按10:2~10:5的重量比充分混合，即得双组份超支化环氧底漆。
2.如权利要求1所述珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法，其特征在于：环氧固化剂的制备中，乙醇、正丁醇、醋酸丁酯的体积比为1:1:1~5:5:1。
3.如权利要求1所述珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法，其特征在于：环氧固化剂的制备中，珍珠岩和膨润土的质量比为1:1~5:1。
4.如权利要求1所述珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法，其特征在于：组分
Figure 162832DEST_PATH_IMAGE002
的制备中，混合溶剂由甲苯、丙酮、醋酸乙酯、醋酸丁酯按4:1:1:1~5:2:2.5:1的质量比混合。
CN201810246653.6A 2018-03-23 2018-03-23 珍珠岩-氰尿酸三聚氰胺固化制备超支化环氧底漆的方法 Expired - Fee Related CN108410319B (zh)

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