CN114213641A - 一种阻燃改性醇酸树脂及其制备方法 - Google Patents

一种阻燃改性醇酸树脂及其制备方法 Download PDF

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CN114213641A
CN114213641A CN202111565066.1A CN202111565066A CN114213641A CN 114213641 A CN114213641 A CN 114213641A CN 202111565066 A CN202111565066 A CN 202111565066A CN 114213641 A CN114213641 A CN 114213641A
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曾小平
田东新
李小平
邹东红
陈豪伟
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Abstract

本发明公开了一种阻燃改性醇酸树脂及其制备方法，阻燃树脂中包括以下成分：含氟二酐30‑60份、多元醇40‑70份、月桂酸40‑50份、有机酸30‑50份、多异氰酸酯30‑50份、异氰酸酯封端的亚胺低聚物15‑35份、二甲亚飒4‑10份、促进剂0.02‑0.3份；本发明采用含氟聚酰亚胺改性醇酸树脂，含氟聚酰亚胺链段提高了树脂的耐高温性能、阻燃性、疏水性，因此本发明具有耐高温、阻燃、耐水的特性。

Description

一种阻燃改性醇酸树脂及其制备方法
技术领域
本发明涉及材料合成技术领域，更具体的说是涉及一种阻燃改性醇酸树脂及其制备方法。
背景技术
醇酸树脂是涂料中应用较广的一种合成树脂，也是目前我国应用最广的合成树脂之一，它价格适中、施工简单、原料来源丰富、酸值低，能溶解于多种有机溶剂，适用于一切木材、金属的表面涂装，对颜料、填料等有较好的润湿和分散性，用其制成的漆膜光亮、附着力强、耐久性好、柔韧性、光泽和丰满度都非常优良，可与多种树脂互溶，改性可制得不同性能的醇酸树脂漆。
发明内容
有鉴于此，本发明提供了一种耐高温、阻燃且耐水的阻燃改性醇酸树脂及其制备方法。
为了实现上述目的，本发明采用如下技术方案：
一种阻燃改性醇酸树脂，按重量份数计，包括以下成分：含氟二酐50-60份、多元醇40-60份、月桂酸40-50份、有机酸30-50份、多异氰酸酯30-40份、异氰酸酯封端的亚胺低聚物15-20份、二甲亚飒4-8份、促进剂0.02-0.1份。
优选的，所述含氟二酐包括6,6’-二-三氟甲基-2,3,3',4'-联苯四甲酸二酐、4,4’-六氟异丙基邻苯二甲酸酐、三蝶烯-4,5-二三氟甲基-2,3,6,7-四甲酸二酐中的至少一种。
优选的，所述多元醇包括季戊四醇、甘油、三、乙二醇、丙二醇、新戊二醇、二乙二醇的至少一种。
优选的，所述有机酸包括对苯二甲酸、间苯二甲酸、叔丁基苯甲酸、己二酸和癸二酸及衍生物的一种或几种混合。
优选的，所述多异氰酸酯包括TDI、HDI、MDI、IPDI、HMDI、H12MDI、TMDI中的至少一种。
优选的，所述促进剂包括碱性金属羧酸盐、有机金属化合物、含磷化合物、胺类中的至少一种；
更优选的，所述促进剂包括醋酸锂、三正丁基磷、辛酸亚锡、环烷酸钴、马来酸二丁基锡、二乙酸二丁基锡、三乙胺、苯甲基缩水甘油醚中的至少一种。
上述阻燃改性醇酸树脂的制备方法，按重量份数计，包括以下步骤：
(1)称量：称取上述阻燃树脂中各原料，备用；
(2)异氰酸酯封端的聚酰亚胺低聚物的合成：通氮气条件下，在反应釜中加入多异氰酸酯、含氟二酐、4-10份溶剂、搅拌并加热至90-120℃，搅拌反应4-6h，反应过程中通过分水装置不断除去反应中产生的水；然后加入二甲亚砜、促进剂，加热至140-200℃保温缩聚3-6h，减压蒸馏出去杂质，即得异氰酸酯封端的聚酰亚胺低聚物；
(3)阻燃树脂的制备：在合成釜中，依次加入月桂酸、有机酸、多元醇、异氰酸酯封端的聚酰亚胺低聚物、8-12份溶剂，通N2升温至150℃，然后以5℃/h的升温速率升温至180～200℃，保温回流2.5h，以10℃/h升温至210～230℃，保温2-3h，降温至100℃以下并加入8-15份溶剂兑稀搅拌0.5h，过滤即制得阻燃改性醇酸树脂。
优选的，所述溶剂包括仲丁酯、乙酸乙酯、丁酯、丙二醇甲醚醋酸酯中的至少一种。
经由上述的技术方案可知，与现有技术相比，本发明具有如下有益效果：与现有技术相比，通常醇酸树脂不具有阻燃效果，而本发明则通过引入酰亚胺结构，提高耐温性，并且进一步提高了阻燃性能，也即，本发明采用含氟聚酰亚胺改性醇酸树脂，含氟聚酰亚胺链段提高了树脂的耐高温性能、阻燃性、疏水性，因此本发明具有耐高温、阻燃、耐水的特性。另根据测试，该树脂的硬度也具有突破，能够用来制备高硬度的产品，可广泛应用于防火墙，家具外漆等领域。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种阻燃改性醇酸树脂，按重量份数计，包括以下成分：三蝶烯-4,5-二三氟甲基-2,3,6,7-四甲酸二酐55份、二乙二醇50份、月桂酸48份、间苯二甲酸40份、MDI40份、异氰酸酯封端的亚胺低聚物20份、二甲亚飒6份、二乙酸二丁基锡0.1份。
实施例2
一种阻燃改性醇酸树脂，按重量份数计，包括以下成分：4,4’-六氟异丙基邻苯二甲酸酐42份、新戊二醇70份、月桂酸40-50份、己二酸40份、TDI50份、异氰酸酯封端的亚胺低聚物35份、二甲亚飒10份、辛酸亚锡0.3份。
实施例3
一种阻燃改性醇酸树脂，按重量份数计，包括以下成分：6,6’-二-三氟甲基-2,3,3',4'-联苯四甲酸二酐30份、季戊四醇40份、月桂酸40份、癸二酸70份、TMDI50份、异氰酸酯封端的亚胺低聚物18份、二甲亚飒5份、三乙胺0.2份。
实施例4
实施例1-3中阻燃剂的制备方法，包括以下步骤：
(1)称量：称取实施例1-3中任一所述的各原料备用；
(2)异氰酸酯封端的聚酰亚胺低聚物的合成：通氮气条件下，在反应釜中加入多异氰酸酯、含氟二酐、10份加氢环保脱芳溶剂D40、搅拌并加热至100℃，搅拌反应5h，反应过程中通过分水装置不断除去反应中产生的水；然后加入二甲亚砜、促进剂，加热至180℃保温缩聚4h，减压蒸馏出去杂质，即得异氰酸酯封端的聚酰亚胺低聚物；
(3)改性醇酸树脂的制备：在合成釜中，依次加入月桂酸、有机酸、多元醇、异氰酸酯封端的聚酰亚胺低聚物、10份加氢环保脱芳溶剂D40，通N2升温至150℃时，然后以5℃/h的升温速率升温至200℃，保温回流2.5h，以10℃/h升温至230℃，保温3h，降温至100℃以下缓慢加入加12份氢环保脱芳溶剂D40份兑稀搅拌1.5h，过滤即制得净阻燃改性醇酸树脂。
实施例5
实施例1-3中阻燃剂的制备方法，包括以下步骤：
(1)称量：称取实施例1-3中任一所述的各原料备用；
(2)异氰酸酯封端的聚酰亚胺低聚物的合成：通氮气条件下，在反应釜中加入多异氰酸酯、含氟二酐、4份乙酸乙酯、搅拌并加热至90℃，搅拌反应4h，反应过程中通过分水装置不断除去反应中产生的水；然后加入二甲亚砜、促进剂，加热至150℃保温缩聚4h，减压蒸馏出去杂质，即得异氰酸酯封端的聚酰亚胺低聚物；
(3)改性醇酸树脂的制备：在合成釜中，依次加入月桂酸、有机酸、多元醇、异氰酸酯封端的聚酰亚胺低聚物、10份乙酸乙酯，通N2升温至150℃时，然后以5℃/h的升温速率升温至180℃，保温回流2h，以10℃/h升温至210℃，保温2h，降温至100℃以下缓慢加入加14份乙酯兑稀搅拌0.5h，过滤即制得净阻燃改性醇酸树脂。
采用实施例5方法制备实施例1-3，实施例1-3相关指标见表1：
表1
外观 粘度(mPa·s) 酸值(mgKOH/g) 羟值(/mgKOH/g)
实施例1 水白 6500 ＜12 121
实施例2 水白 5000 ＜12 150
实施例3 水白 4500 ＜12 180
将实施例1-3与市售TDI三聚体固化剂按照-OH：-NCO＝1:1配漆，喷涂于木器之上，漆膜厚度100微米，测试漆膜性能见表2：
表2
Figure BDA0003421776780000051
以上可以看出，实例1硬度较高，实例2，3韧性较好。
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言，由于其与实施例公开的方法相对应，所以描述的比较简单，相关之处参见方法部分说明即可。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (8)

1.一种阻燃改性醇酸树脂，其特征在于，按重量份数计，包括以下成分：含氟二酐30-60份、多元醇40-70份、月桂酸40-50份、有机酸30-50份、多异氰酸酯30-50份、异氰酸酯封端的亚胺低聚物15-35份、二甲亚飒4-10份、促进剂0.02-0.3份。
2.根据权利要求1所述的一种阻燃改性醇酸树脂，其特征在于，所述含氟二酐包括6,6’-二-三氟甲基-2,3,3',4'-联苯四甲酸二酐、4,4’-六氟异丙基邻苯二甲酸酐、三蝶烯-4,5-二三氟甲基-2,3,6,7-四甲酸二酐中的至少一种。
3.根据权利要求1所述的一种阻燃改性醇酸树脂，其特征在于，所述多元醇包括季戊四醇、甘油、三、乙二醇、丙二醇、新戊二醇、二乙二醇的至少一种。
4.根据权利要求1所述的一种阻燃改性醇酸树脂，其特征在于，所述有机酸包括对苯二甲酸、间苯二甲酸、叔丁基苯甲酸、己二酸，癸二酸及衍生物的一种或几种混合。
5.根据权利要求1所述的一种阻燃改性醇酸树脂，其特征在于，所述多异氰酸酯包括TDI、HDI、MDI、IPDI、HMDI、H12MDI、TMDI中的至少一种。
6.根据权利要求1所述的一种阻燃改性醇酸树脂，其特征在于，所述促进剂包括碱性金属羧酸盐、有机金属化合物、含磷化合物、胺类中的至少一种。
7.一种阻燃改性醇酸树脂的制备方法，其特征在于，按重量份数计，包括以下步骤：
(1)称量：称取权利要求1-6任一所述阻燃树脂中各原料，备用；
(2)异氰酸酯封端的聚酰亚胺低聚物的合成：通氮气条件下，在反应釜中加入多异氰酸酯、含氟二酐、4-10份溶剂、搅拌并加热至90-120℃，搅拌反应4-6h，反应过程中通过分水装置不断除去反应中产生的水；然后加入二甲亚砜、促进剂，加热至140-200℃保温缩聚3-6h，减压蒸馏出去杂质，即得异氰酸酯封端的聚酰亚胺低聚物；
(3)阻燃树脂的制备：在合成釜中，依次加入月桂酸、有机酸、多元醇、异氰酸酯封端的聚酰亚胺低聚物、8-12份溶剂，通N2升温至150℃，然后以5℃/h的升温速率升温至180～200℃，保温回流2.5h，以10℃/h升温至210～230℃，保温2-3h，降温至100℃以下并加入8-15份溶剂兑稀搅拌0.5h，过滤即制得阻燃改性醇酸树脂。
8.根据权利要求7所述的一种阻燃改性醇酸树脂的制备方法，其特征在于，所述溶剂包括仲丁酯、乙酸乙酯、丁酯、丙二醇甲醚醋酸酯中的至少一种。
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CN115785776A (zh) * 2022-12-07 2023-03-14 大使涂料(安徽)有限公司 一种含氟醇酸环保涂料及其制备方法

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CN110818887A (zh) * 2019-12-06 2020-02-21 合众（佛山）化工有限公司 一种净味抗划伤改性醇酸树脂的制备方法

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CN110818887A (zh) * 2019-12-06 2020-02-21 合众（佛山）化工有限公司 一种净味抗划伤改性醇酸树脂的制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115785776A (zh) * 2022-12-07 2023-03-14 大使涂料(安徽)有限公司 一种含氟醇酸环保涂料及其制备方法
CN115785776B (zh) * 2022-12-07 2023-10-13 大使涂料(安徽)有限公司 一种含氟醇酸环保涂料及其制备方法

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