CN104312394B - 一种阻燃醇酸树脂涂料及其制备方法 - Google Patents

一种阻燃醇酸树脂涂料及其制备方法 Download PDF

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CN104312394B
CN104312394B CN201410628525.XA CN201410628525A CN104312394B CN 104312394 B CN104312394 B CN 104312394B CN 201410628525 A CN201410628525 A CN 201410628525A CN 104312394 B CN104312394 B CN 104312394B
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宋美娟
张宝同
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SHANDONG WUZHOU DETECTION Co Ltd
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Abstract

本发明公开了一种阻燃醇酸树脂涂料及其制备方法，质量份数组成为：醇酸树脂80‑90份，钛白粉12‑15份，十溴二苯醚3‑5份，六溴环十二烷2‑3份，磷酸三苯酯0.5‑2份，硼酸锌0.5‑2份，滑石粉0.2‑1份，氢氧化镁0.5‑1.5份，抗氧剂0.1‑0.2份，流平剂0.3‑0.5份，消泡剂0.3‑0.5份，分散剂3‑4份和二甲苯丁酯混合溶剂10‑15份。本发明的有益效果是：阻燃效果好，阻燃剂添加量少；制备工艺简单，操作方便。

Description

一种阻燃醇酸树脂涂料及其制备方法
技术领域
本发明涉及化工技术领域，特别涉及一种阻燃醇酸树脂涂料及其制备方法。
背景技术
醇酸树脂涂料具有漆膜附着力好、光亮、丰满等特点，一般是由油脂（或油酸）、多元醇、多元酸等有机化工原料经缩合化学反应制得的有机高分子树脂。但是在应用中醇酸树脂涂料的阻燃效果不好，不能满足使用要求。
发明内容
为了满足改善醇酸树脂涂料阻燃性能的需求，本发明提供了一种阻燃醇酸树脂涂料。
为了实现上述发明目的，本发明提供了一种阻燃醇酸树脂涂料，质量份数组成为：醇酸树脂80-90份，钛白粉12-15份，十溴二苯醚3-5份，六溴环十二烷2-3份，磷酸三苯酯0.5-2份，硼酸锌0.5-2份，滑石粉0.2-1份，氢氧化镁0.5-1.5份，抗氧剂0.1- 0.2份，流平剂0.3-0.5份，消泡剂0.3-0.5份，分散剂3-4份和二甲苯丁酯混合溶剂10-15份。
所述醇酸树脂由桐油酸、蓖麻油酸和菜籽油酸混合物30.0-40.0份，甘油和季戊四醇的混合物14-20.0份，间苯二甲酸13-15份以及带水剂4-6份组成，所述桐油酸、蓖麻油酸和菜籽油酸质量比为1-2：0.5-1.5:2-3，所述甘油：季戊四醇的质量比为1-3:2-5。
所述阻燃醇酸树脂涂料质量份数组成为：醇酸树脂83份，钛白粉12份，十溴二苯醚4份 六溴环十二烷3份，磷酸三苯酯1份，硼酸锌2份，滑石粉1份，氢氧化镁1份，抗氧剂0.2份，流平剂0.3份，消泡剂0.3份，分散剂3份和二甲苯丁酯混合溶剂12份。
所述醇酸树脂由桐油酸、蓖麻油酸和菜籽油酸混合物40.0份，甘油和季戊四醇的混合物18.0份，间苯二甲酸13份以及带水剂5份组成，所述桐油酸、蓖麻油酸和菜籽油酸质量比为2：1: 3，所述甘油：季戊四醇的质量比为3:4。
本发明还提供一种阻燃醇酸树脂涂料的制备方法，包括以下步骤：
（1）在带水剂的存在下，用桐油酸、蓖麻油酸和菜籽油酸、间苯二甲酸、甘油和季戊四醇的混合物进行酯化反应一段时间后，降低反应温度至190℃，反应到酸值≤10mgKOH/g时停止加热，降温至室温，出料，即得醇酸树脂；
（2）按质量份数取醇酸树脂钛白粉，分散剂研磨至800目，得混合物1；
（3）按质量份数取十溴二苯醚、六溴环十二烷，磷酸三苯酯，硼酸锌，滑石粉，氢氧化镁，抗氧剂，流平剂，消泡剂混合均匀研磨至800目，得混合物2；
（4）将步骤（2）得到的混合物1和步骤（3）得到的混合物2混合均匀研磨30-60分钟，按质量份数加入二甲苯丁酯混合溶剂混合均匀即可得到阻燃醇酸树脂涂料。
本发明实施例提供的技术方案带来的有益效果是：
1、阻燃效果好，阻燃剂添加量少；
2、制备工艺简单，操作方便。
具体实施方式
针对醇酸树脂阻燃性差的问题，本发明提供了一种阻燃醇酸树脂涂料，具有良好的阻燃效果。
流平剂：东莞市易立安化工科技有限公司，EL-2503。
分散剂：东莞市易立安化工科技有限公司，EL-2208。
消泡剂：东莞市易立安化工科技有限公司，EL-2602。
抗氧剂：上海仙邦化学专业经销涂料抗氧剂，WD-3024。
二甲苯丁酯混合溶剂:扬州安平化工有限公司 二甲苯和醋酸丁酯体积百分比各占50%
实施例1
（1）在四口烧瓶中，在带水剂16.7克二甲苯的存在下，加入156.6克桐油酸、蓖麻油酸和菜籽油酸混合物，74.8克间苯二甲酸、47.7克甘油和季戊四醇的混合物进行酯化反应一段时间后，降低反应温度至190℃，反应到酸值≤10mgKOH/g时停止加热，降温至室温，出料，即得醇酸树脂；其中桐油酸、蓖麻油酸、菜籽油酸质量比为2：1: 3，甘油和季戊四醇质量比为3:2；
（2）按质量比取醇酸树脂83g，钛白粉12g，分散剂3g研磨至800目，得混合物1；
(3) 按质量份数取十溴二苯醚4g份、六溴环十二烷3g，磷酸三苯酯1g，硼酸锌2g，滑石粉1g，氢氧化镁1g，抗氧剂0.2 g，流平剂0.3g，消泡剂0.3g混合均匀研磨至800目，得混合物2；
（4）将步骤（2）得到的混合物1和步骤（3）得到的混合物2混合均匀研磨30-60分钟，按质量份数加入二甲苯丁酯混合溶剂12g混合均匀即可得到阻燃醇酸树脂涂料。
实施例2
（1）在四口烧瓶中，在带水剂16.6克二甲苯的存在下，加入158.8克桐油酸、蓖麻油酸和菜籽油酸混合物，66.5克间苯二甲酸、51克甘油和季戊四醇的混合物进行酯化反应一段时间后，降低反应温度至190℃，反应到酸值≤10mgKOH/g时停止加热，降温至室温，出料，即醇酸树脂；其中桐油酸、蓖麻油酸、菜籽油酸质量比为1：0.5:2，甘油和季戊四醇质量比为1:5；
（2）按质量比取醇酸树脂90g，钛白粉15g，分散剂4g研磨至800目，得混合物1；
(3) 按质量份数取十溴二苯醚3g份、六溴环十二烷2g，磷酸三苯酯2g，硼酸锌1g，滑石粉0.2g，氢氧化镁0.5g，抗氧剂0.2 g，流平剂0.4g，消泡剂0.5g混合均匀研磨至800目，得混合物2；
（4）将步骤（2）得到的混合物1和步骤（3）得到的混合物2混合均匀研磨30-60分钟，按质量份数加入二甲苯丁酯混合溶剂15g混合均匀即可得到阻燃醇酸树脂涂料。
实施例3
（1）在四口烧瓶中，在带水剂15.6克二甲苯的存在下，加入157.5克桐油酸、蓖麻油酸和菜籽油酸混合物，72.30克间苯二甲酸、50克甘油和季戊四醇的混合物进行酯化反应一段时间后，降低反应温度至190℃，反应到酸值≤10mgKOH/g时停止加热，降温至室温，出料，即醇酸树脂；其中桐油酸、蓖麻油酸、菜籽油酸质量比为1：1.5: 3，甘油和季戊四醇质量比为2:3；
（2）按质量比取醇酸树脂80g，钛白粉13g，分散剂4g研磨至800目，得混合物1；
(3) 按质量份数取十溴二苯醚5g份、六溴环十二烷3g，磷酸三苯酯0.5g，硼酸锌0.5g，滑石粉0.8g，氢氧化镁1.5g，抗氧剂0.1 g，流平剂0.5g，消泡剂0.4g混合均匀研磨至800目，得混合物2；
（4）将步骤（2）得到的混合物1和步骤（3）得到的混合物2混合均匀研磨30-60分钟，按质量份数加入二甲苯丁酯混合溶剂10g混合均匀即可得到阻燃醇酸树脂涂料。
阻燃效果评价：
将普通的醇酸树脂涂料和上述实施例1-3制备的阻燃醇酸树脂涂料在玻璃板上涂膜，干燥后得到约2mm厚涂膜，将涂膜从玻璃板上取下，按照国家标准GB/T2406进行氧指数测定，测得结果列于下表：
由表中数据可知，本发明制备的阻燃醇酸树脂涂料其氧指数比未阻燃的醇酸树脂的高很多，具有优异的阻燃性能。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，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 (4)

1.一种阻燃醇酸树脂涂料，其特征在于，质量份数组成为：醇酸树脂80-90份，钛白粉12-15份，十溴二苯醚3-5份，六溴环十二烷2-3份，磷酸三苯酯0.5-2份，硼酸锌0.5-2份，滑石粉0.2-1份，氢氧化镁0.5-1.5份，抗氧剂0.1-0.2份，流平剂0.3-0.5份，消泡剂0.3-0.5份，分散剂3-4份，二甲苯和醋酸丁酯混合溶剂10-15份；
所述醇酸树脂由桐油酸、蓖麻油酸和菜籽油酸混合物30.0-40.0份，甘油和季戊四醇的混合物14-20.0份，间苯二甲酸13-15份以及带水剂4-6份制成，所述桐油酸、蓖麻油酸和菜籽油酸质量比为1-2：0.5-1.5:2-3，所述甘油：季戊四醇的质量比为1-3:2-5。
2.根据权利要求1所述的阻燃醇酸树脂涂料，其特征在于，质量份数组成为：醇酸树脂83份，钛白粉12份，十溴二苯醚4份，六溴环十二烷3份，磷酸三苯酯1份，硼酸锌2份，滑石粉1份，氢氧化镁1份，抗氧剂0.2份，流平剂0.3份，消泡剂0.3份，分散剂3份，二甲苯和醋酸丁酯混合溶剂12份。
3.根据权利要求1或2所述的阻燃醇酸树脂涂料，其特征在于，所述醇酸树脂由桐油酸、蓖麻油酸和菜籽油酸混合物40.0份，甘油和季戊四醇的混合物18.0份，间苯二甲酸13份以及带水剂5份制成，所述桐油酸、蓖麻油酸和菜籽油酸质量比为2：1:3，所述甘油：季戊四醇的质量比为3:4。
4.一种权利要求1-3任一所述的阻燃醇酸树脂涂料的制备方法，其特征在于，包括以下步骤：
(1)在带水剂的存在下，用桐油酸、蓖麻油酸和菜籽油酸、间苯二甲酸、甘油和季戊四醇的混合物进行酯化反应一段时间后，降低反应温度至190℃，反应到酸值≤10mgKOH/g时停止加热，降温至室温，出料，即得醇酸树脂；
(2)按质量份数取醇酸树脂、钛白粉和分散剂研磨至800目，得混合物1；
(3)按质量份数取十溴二苯醚、六溴环十二烷，磷酸三苯酯，硼酸锌，滑石粉，氢氧化镁，抗氧剂，流平剂，消泡剂混合均匀研磨至800目，得混合物2；
(4)将步骤(2)得到的混合物1和步骤(3)得到的混合物2混合均匀研磨30-60分钟，按质量份数加入二甲苯和醋酸丁酯混合溶剂混合均匀即可得到阻燃醇酸树脂涂料。
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