CN109354937A - 一种氟碳涂料用柔性固化剂及其制备方法 - Google Patents

一种氟碳涂料用柔性固化剂及其制备方法 Download PDF

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CN109354937A
CN109354937A CN201811125284.1A CN201811125284A CN109354937A CN 109354937 A CN109354937 A CN 109354937A CN 201811125284 A CN201811125284 A CN 201811125284A CN 109354937 A CN109354937 A CN 109354937A
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张志忠
赵凯
杜存山
祝和权
南阳
王涛
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JIANGSU PROVINCE RESEARCH INSTITUTE OF CHEMICAL INDUSTRY Co Ltd
Metals and Chemistry Research Institute of CARS
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Abstract

本发明提供一种氟碳涂料用柔性固化剂及其制备方法，属于化工涂料领域，该固化剂包括的组分有改性低不饱和度高分子量聚醚多元醇、聚酯多元醇、脂肪族异氰酸酯、稀释剂和催化剂，该固化剂制备方法包括如下步骤：先将改性低不饱和度高分子量聚醚多元醇、聚酯多元醇投入反应釜，搅拌均匀，升温并脱水一段时间，然后在搅拌过程中加入脂肪族异氰酸酯，搅拌后将催化剂缓慢滴加到反应釜中，控制温度，恒温反应一段时间，最后加入稀释剂，搅拌均匀，检测NCO达到设定值时停止反应，然后真空脱泡，出料即得固化剂。与常规脂肪族固化剂相比，本发明制备的固化剂与氟碳树脂配制的涂料具有更好的拉伸强度、断裂伸长率以及耐低温性能。

Description

一种氟碳涂料用柔性固化剂及其制备方法
技术领域
本发明属于化工涂料领域，具体涉及一种氟碳涂料用柔性固化剂及其制备方法。
背景技术
目前我国高速铁路一般采用无砟轨道，因而需使用大量的混凝土桥梁，混凝土桥梁中含有大量钢结构，但是钢结构的防腐维护已成为无砟轨道使用中需要面对的重要问题。氟碳涂料是一种用于钢结构防腐的面漆，因其独特的F-C键结构，具有优异的耐老化性能，但是现有的氟碳涂料由于自身的结构特性以及固化剂的问题，形成的涂层呈现脆性，涂层的断裂伸长率为0-50％，耐低温性能也较差，尤其在北方的寒冷天气下，特别容易开裂，大大增加了维护难度及维护成本。为适应混凝土桥梁中钢结构表面的保护涂装，需使涂层具有一定的柔性，目前市场上的氟碳树脂通常不具有制备柔性涂层的功能，因此急需一种提高氟碳涂料拉伸强度、断裂伸长率和耐低温性能的柔性固化剂。
发明内容
为了解决现有技术中存在的涂料耐低温性能差、柔韧性不足、高强度下伸长率不高的问题，本发明提供一种氟碳涂料用柔性固化剂及其制备方法，具有提高氟碳涂料拉伸强度、断裂伸长率、耐低温性能的优点。
本发明提供了如下的技术方案：
一种氟碳涂料用柔性固化剂及其制备方法，包括以下组分：改性低不饱和度高分子量聚醚多元醇100重量份、聚酯多元醇10-20重量份、脂肪族异氰酸酯30-45重量份、稀释剂20-30重量份和催化剂0.02-0.04重量份。
优选的，所述改性低不饱和度高分子量聚醚多元醇由分子量为6000-10000的二官能度多元醇、分子量为6000-10000的三官能度多元醇、分子量为2000-4000的聚四氢呋喃醚及脂肪族异氰酸酯反应合成，所述二官能度多元醇、三官能度多元醇、聚四氢呋喃醚和脂肪族异氰酸酯的重量份比为100:60:20:3。
优选的，制备改性低不饱和度高分子量聚醚多元醇的反应温度为80-90℃，反应时间为0.5-2h。
优选的，所述聚酯多元醇为分子量为2000-4000的聚己内酯二醇或聚碳酸酯二醇。
优选的，所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯或六亚甲基二异氰酸酯。
优选的，所述稀释剂为乙酸乙酯、乙酸丁酯和二甲苯中的一种。
优选的，所述催化剂为乙酸丁酯稀释有机锡催化剂或有机铋催化剂所复配的催化剂。
一种氟碳涂料用柔性固化剂的制备方法，包括如下步骤：
S1：先将改性低不饱和度高分子量聚醚多元醇、聚酯多元醇投入反应釜，搅拌均匀，升温至一定温度并脱水一段时间；
S2：然后在搅拌过程中加入脂肪族异氰酸酯，搅拌10min后将稀释的催化剂按量缓慢滴加到反应釜中，控制温度，恒温反应一段时间；
S3：最后加入稀释剂，搅拌0.5-1h，检测NCO达到设定值时停止反应，然后真空脱泡0.5h，出料即得固化剂。
优选的，S1步骤中的脱水温度为110-120℃，脱水时间为1-1.5h。
优选的，S2步骤中将催化剂按量缓慢滴加到反应釜中，控制温度在90-95℃，恒温反应时间为4-5h。
本发明的有益效果是：
(1)本发明采用脂肪族异氰酸酯作为原料，由于其不含苯环，制得的固化剂具有较好耐黄变性能。本发明还采用改性低不饱和度高分子量聚醚多元醇、聚酯多元醇为原料，制得的固化剂中的柔性链段较多，与氟碳树脂制得的涂层具有较好的拉伸强度、断裂伸长率以及耐低温性能。
(2)将本发明制得的固化剂与氟碳树脂复合使用，喷涂在混凝土、钢结构等表面上，形成的涂层具有柔性，涂层的拉伸强度为7-15MPa，断裂伸长率为170-250％，即使在低温条件下还具有一定的柔韧性及伸长率，保证面漆完整不开裂，可以对混凝土以及钢结构提供耐久性保护。
具体实施方式
下面通过实施例对本发明内容进一步说明，具体如下：
实施例1
改性低不饱和度高分子量聚醚多元醇的制备：将100重量份分子量为6000-10000的二官能度多元醇、60重量份分子量为6000-10000的三官能度多元醇、20重量份分子量为2000-4000的聚四氢呋喃醚及3重量份脂肪族异氰酸酯反应合成改性低不饱和度高分子量聚醚多元醇，反应温度为80-90℃，反应时间为0.5-2h。
固化剂的制备：将100重量份改性低不饱和度高分子量聚醚多元醇、20重量份聚碳酸酯二醇投入反应釜，搅拌均匀，升温至110-120℃脱水1-1.5h，然后在搅拌过程中加入40重量份异佛尔酮二异氰酸酯，搅拌10min后将稀释的催化剂按量缓慢滴加入反应釜中，温度控制在90-95℃，恒温反应4-5h，最后加入乙酸丁酯，搅拌0.5h，检测NCO达到设定值时停止反应，真空脱泡0.5h，出料即得固化剂。
实施例2
固化剂的制备：将100重量份实施例1中制备的改性低不饱和度高分子量聚醚多元醇、15重量份聚己内酯二醇投入反应釜，搅拌均匀，升温至110-120℃脱水1-1.5h，然后在搅拌过程中加入30重量份六亚甲基二异氰酸酯，搅拌10min后将稀释的催化剂按量缓慢滴加入反应釜中，温度控制在90-95℃，恒温反应4-5h，最后加入乙酸乙酯，搅拌0.5h，检测NCO达到设定值时停止反应，真空脱泡0.5h，出料即得固化剂。
实施例3
固化剂的制备：将100重量份实施例1中制备的改性低不饱和度高分子量聚醚多元醇、20重量份聚己内酯二醇投入反应釜，搅拌均匀，升温至110-120℃脱水1-1.5h，然后在搅拌过程中加入44重量份异佛尔酮二异氰酸酯，搅拌10min后将稀释的催化剂按量缓慢滴加入反应釜中，温度控制在90-95℃，恒温反应4-5h，最后加入二甲苯，搅拌0.5h，检测NCO达到设定值时停止反应，真空脱泡0.5h，出料即得固化剂。
实验结果
拉伸强度、断裂伸长率测定：将日本旭硝子公司的LUMIFLON氟碳树脂与常规脂肪族固化剂及实施例1至3所制备的固化剂按重量份比6:8-12复配，并制成自由膜，自由膜厚度200-500μm，在温度23±2℃，相对湿度50±10％的环境下，养护24h，然后放入105±2℃烘箱中下保持1h，取出，自然冷却后，将自由膜裁成GB/T 528-2009规定的哑铃状Ⅰ型试样，在(250±50)mm/min移动速度的试验机上对自由膜拉伸强度、拉断伸长率进行测定，测试结果见表1。
低温柔性测定：将日本旭硝子公司的LUMIFLON氟碳树脂与常规脂肪族固化剂及实施例1至3所制备的固化剂按重量份比6:8-12复配，刷涂在马口铁板表面，涂层固化后干膜厚度30-40μm，在23±2℃、相对湿度50±5％环境条件下养护24h后放入105±2℃的烘箱中烘干1h，取出，自然冷却后，将试样放置在温度为-35℃的低温箱内保温2h，使用GB/T 6742规定中2mm弯曲试验仪进行弯折，若-35℃下断裂即为差，不断裂即为好，测试结果见表1。
表1
实验结果表明，相对于常规脂肪族固化剂，本发明制备的固化剂与氟碳树脂制得的涂层具有更好的拉伸强度、断裂伸长率和耐低温性能。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (10)

1.一种氟碳涂料用柔性固化剂，其特征在于，包括以下组分：改性低不饱和度高分子量聚醚多元醇100重量份、聚酯多元醇10-20重量份、脂肪族异氰酸酯30-45重量份、稀释剂20-30重量份和催化剂0.02-0.04重量份。
2.根据权利要求1所述的一种氟碳涂料用柔性固化剂，其特征在于，所述改性低不饱和度高分子量聚醚多元醇由分子量为6000-10000的二官能度多元醇、分子量为6000-10000的三官能度多元醇、分子量为2000-4000的聚四氢呋喃醚及脂肪族异氰酸酯反应合成，所述二官能度多元醇、三官能度多元醇、聚四氢呋喃醚和脂肪族异氰酸酯的重量份比为100:60:20:3。
3.根据权利要求2所述的一种氟碳涂料用柔性固化剂，其特征在于，制备改性低不饱和度高分子量聚醚多元醇的反应温度为80-90℃，反应时间为0.5-2h。
4.根据权利要求1所述的一种氟碳涂料用柔性固化剂，其特征在于，所述聚酯多元醇为分子量为2000-4000的聚己内酯二醇或聚碳酸酯二醇。
5.根据权利要求1所述的一种氟碳涂料用柔性固化剂，其特征在于，所述脂肪族异氰酸酯为异佛尔酮二异氰酸酯或六亚甲基二异氰酸酯。
6.根据权利要求1所述的一种氟碳涂料用柔性固化剂，其特征在于，所述稀释剂为乙酸乙酯、乙酸丁酯和二甲苯中的一种。
7.根据权利要求1所述的一种氟碳涂料用柔性固化剂，其特征在于，所述催化剂为乙酸丁酯稀释有机锡催化剂或有机铋催化剂所复配的催化剂。
8.一种氟碳涂料用柔性固化剂的制备方法，其特征在于，包括如下步骤：
S1：先将改性低不饱和度高分子量聚醚多元醇、聚酯多元醇投入反应釜，搅拌均匀，升温至一定温度并脱水一段时间；
S2：然后在搅拌过程中加入脂肪族异氰酸酯，搅拌10min后将稀释的催化剂按量缓慢滴加到反应釜中，控制温度，恒温反应一段时间；
S3：最后加入稀释剂，搅拌0.5-1h，检测NCO达到设定值时停止反应，然后真空脱泡0.5h，出料即得固化剂。
9.根据权利要求8所述的一种氟碳涂料用柔性固化剂的制备方法，其特征在于，S1步骤中的脱水温度为110-120℃，脱水时间为1-1.5h。
10.根据权利要求8所述的一种氟碳涂料用柔性固化剂的制备方法，其特征在于，S2步骤中将催化剂按量缓慢滴加到反应釜中，控制温度在90-95℃，恒温反应时间为4-5h。
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