CN112048070A - 端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法 - Google Patents
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Abstract
本发明公开了一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法。该分散剂是利用环氧大豆油分子链上的环氧基与三(羟甲基)氨基甲烷分子上氨基发生开环反应，然后再与环氧丙醇发生反应制备得到的。所制得的超分散剂分子结构末端含有大量的活性羟基，这些活性羟基可与木塑填料表面形成多点锚固，通过这些多点“锚固”作用将大豆油分子链牢牢镶嵌在填料表面，提高填料在聚烯烃树脂中的分散性。本发明具有制备工艺简单、生产成本低、机械强度高、环境污染小等优良特性，不仅能提高木塑复合材料的使用寿命，还能大幅度提高木塑复合材料的力学性能。
Description
技术领域
本发明属于木塑门窗复合材料用加工助剂生产技术领域，尤其涉及一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法。
背景技术
木塑门窗是将木材和塑料两种材料的优点结合起来的一种木塑复合材料，是目前国内最好的窗户。作为窗户用的木塑复合材料是近几年迅速发展起来的一种新型材料，它是由60％植物纤维（如木纤维粉、麻纤维粉、竹纤维粉、草纤维粉、糠皮粉或秸秆纤维粉等）及无机填料（如碳酸钙、滑石粉及石英粉等）、30％高分子树脂（如聚丙烯、聚乙烯或聚氯乙烯等）及10％专用助剂（如表面处理剂、增韧剂、润滑剂等），经机械混合、熔融分散、成型加工等工序制得的一种新型复合材料。木塑复合材料具有制备简单方便、生产成本低廉、机械强度高、保温阻音、防水阻燃、寿命长等优良的特性，广泛用于建材、家具、物流包装等行业。但由于强极性植物纤维和非极性的聚烯烃树脂相容性差，界面结合不紧密，导致制品品质下降。如何提高纤维在聚烯烃树脂中的分散性，以及树脂和纤维之间的界面相容性，是提高木塑复合材料性能的关键，也是木塑产业和木塑门窗产业能否快速发展的关键因素。因此，研究开发一种对纤维和无机粉体分散性好，并与树脂有较好相容性的木塑相容分散剂尤为重要。
目前木塑复合材料界面相容改性常用的方法有偶联剂法、润滑剂法、超分散剂法及相容剂法等；主要的改性剂有硬脂酸、白油、硅烷偶联剂、铝烷偶联剂和钛酸酯偶联剂等，这些改性剂主要是通过化学反应来减少植物纤维、玻璃纤维或无机粉体等填料表面的羟基数目，在填料/聚烯烃树脂之间建立物理和化学交联，并在填料表面形成一层憎水性薄膜，从而提高其与聚烯烃树脂的界面相容性和促进填料的分散，防止填料团聚，提高制品的抗冲击强度及加工流变性能。
超分散剂又名超级分散剂，是一种特殊的表面活性剂，其分子结构中含有锚固基团和溶剂化链段。与传统分散剂的区别表现在:①是锚固基团的引进，它们通过离子键、共价键、氢键及范德化力等相互作用，紧紧吸附在纤维和无机粉体表面，且多为不可逆吸附，很难解吸；②主链式溶剂化链亲油基团，与树脂有良好的相容性，且具有较好的伸展构想，在纤维和无机粉体表面形成足够厚的保护层。当溶剂化链段很好的溶解和适当的展开时，位阻稳定作用得到加强，大大提高了溶剂化链的有效利用率，从而提高聚烯烃树脂与填料粉体的结合力。目前超分散剂在木塑复合材料中的应用，已有不少文献专利报道，如“木塑复合材料用超支化分散剂的制备方法”(CN201110046643.6)、“一种超支化分散剂的制备方法及其应用”(CN201510415798.0)、“废剑麻纤维用柔性链超分散剂及其制备方法”(CN200910114226.3)、“多乙烯多胺-接枝聚羟基酸酯超分散剂及制备方法”(CN201010045605.4)等，所有这些研究均表明了超分散剂能够大幅度提高木塑复合材料的力学性能。
基于此，本发明提出一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法。该超分散剂主要是利用环氧大豆油、三(羟甲基)氨基甲烷、环氧丙醇等为原料反应得到的，其分子结构末端含有大量的活性羟基，这些活性羟基可与木塑填料（如木粉、玻璃纤维、碳酸钙粉体等）表面形成多点锚固作用，并在填料表面形成一层包覆层。将该超分散剂用于由聚烯烃树脂（如聚乙烯、聚丙烯、聚氯乙烯等）、填料等共混改性制备得到的木塑门窗复合材料，具有制备简单方便、生产成本低廉、机械强度高及环境污染小等优点，并能大大提高木塑门窗复合材料的力学性能，降低吸水率和收缩膨胀率，延长材料的使用寿命。
发明内容
本发明的目的是提供一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法。该超分散剂能有效提高木塑门窗复合材料的强度和韧性、降低吸水率和收缩膨胀率，减少环境污染，生态环保。
本发明的目的通过以下技术方案来实现：
一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法，具体步骤为：
(1)在250mL三口烧瓶中加入20~25g环氧大豆油、20~25 g三(羟甲基)氨基甲烷、0.2~0.4g四氟硼酸和100~120g异丙醇，在65~75℃下搅拌反应25~28h后，蒸馏除去异丙醇。反应物用饱和硫酸钠溶液洗涤，除去未完全反应的三(羟甲基)氨基甲烷，干燥后得到粘稠状棕黄色液体，即为大豆油多元醇。
(2)称取80~100mL四氢呋喃和50~80 uL甲醇钾加入步骤(1)制得的大豆油多元醇中，在氮气保护下于50~60℃搅拌1h；然后加入20~30mL二氧六环，升高温度到95℃后，缓慢滴加8~10mL环氧丙醇，继续恒温搅拌反应5~6h，待反应结束后冷至室温，用50~70mL甲醇反复洗涤3次，所得产物置于60℃的真空干燥箱中烘干10h，即制得端羟基超支化聚酯接枝环氧大豆油超分散剂，其分子量为2500~3000。
本发明的端羟基超支化聚酯接枝环氧大豆油超分散剂应用于木塑门窗复合材料的填料表面改性，所述填料包括木粉、竹粉、玻璃纤维、碳酸钙和滑石粉。
本发明的超分散剂的分子结构中含有多个羟基“锚固”基团，可在木纤维、玻璃纤维、碳酸钙粉体等表面形成多点“锚固”作用，对木纤维、玻璃纤维、碳酸钙粉体等具有优异的分散性能。用于改性聚烯烃（如聚丙烯、聚乙烯或聚氯乙烯等）树脂、木纤维、竹纤维、玻璃纤维、碳酸钙粉体、滑石粉等共混体系制备得到木塑门窗复合材料，由于该超分散剂分子结构中的大豆油柔性长链可以与聚烯烃树脂分子链发生物理缠结作用，有利于改善木纤维、玻璃纤维、碳酸钙粉体等与聚烯烃树脂之间的界面相容性，还有利于提高木塑门窗复合材料的力学性能，降低吸水率和收缩膨胀率，而且能改善复合材料的润滑度和表面光洁度。
附图说明
图1为本发明制备的端羟基超支化聚酯接枝环氧大豆油超分散剂的分子结构式。
具体实施方式
实施例所用的主要原料如下：环氧大豆油，工业级(酸值 0.6mg KOH /g，环氧值0. 65%)；三(羟甲基)氨基甲烷，化学纯；四氟硼酸，分析纯；环氧丙醇，化学纯；其余为市售化学纯试剂。
实施例1：
(1)在250mL三口烧瓶中加入20g环氧大豆油、20g三(羟甲基)氨基甲烷、0.2g四氟硼酸和100g异丙醇，在70℃下搅拌反应25h后，蒸馏除去异丙醇。反应物用饱和硫酸钠溶液洗涤，除去未完全反应的三(羟甲基)氨基甲烷，干燥后得到粘稠状棕黄色液体，即为大豆油多元醇。
(2)称取80mL四氢呋喃和50uL甲醇钾加入步骤(1)制得的大豆油多元醇中，在氮气保护下于60℃搅拌1h；然后加入20mL二氧六环，升高温度到95℃后，缓慢滴加8mL环氧丙醇，继续恒温搅拌反应6h。待反应结束后冷至室温，用50mL甲醇溶液反复洗涤3次，产物置于60℃的真空干燥箱中烘干10h，即制得端羟基超支化聚酯接枝环氧大豆油超分散剂，其分子量为2500~3000。
实施例2：
(1)在250mL三口烧瓶中加入23g环氧大豆油、23 g三(羟甲基)氨基甲烷、0.3g四氟硼酸和110g异丙醇，在70℃下搅拌反应25h后，蒸馏除去异丙醇。反应物用饱和硫酸钠溶液洗涤，除去未完全反应的三(羟甲基)氨基甲烷，干燥后得到粘稠状棕黄色液体，即为大豆油多元醇。
(2)称取90mL四氢呋喃和60uL甲醇钾加入步骤(1)制得的大豆油多元醇中，在氮气保护下于60℃搅拌1h；然后加入25mL二氧六环，升高温度到95℃后，缓慢滴加9mL环氧丙醇，继续恒温搅拌反应6h。待反应结束后冷至室温，用50mL甲醇反复洗涤3次，产物置于60℃的真空干燥箱中烘干10h，即制得端羟基超支化聚酯接枝环氧大豆油超分散剂，其分子量为2500~3000。
实施例3：
(1)在250mL三口烧瓶中加入25g环氧大豆油、25g三(羟甲基)氨基甲烷、0.4g四氟硼酸和120g异丙醇，在70℃下搅拌反应25h后，蒸馏除去异丙醇。反应物用饱和硫酸钠溶液洗涤，除去未完全反应的三(羟甲基)氨基甲烷，干燥后得到粘稠状棕黄色液体，即为大豆油多元醇。
(2)称取100mL四氢呋喃和70uL甲醇钾加入步骤(1)制得的大豆油多元醇中，在氮气保护下于60℃搅拌1h；然后加入30mL二氧六环，升高温度到95℃后，缓慢滴加10mL环氧丙醇，继续恒温搅拌反应6h。待反应结束后冷至室温，用70mL甲醇反复洗涤3次，产物置于60℃的真空干燥箱中烘干10h，即制得端羟基超支化聚酯接枝环氧大豆油超分散剂，其分子量为2500~3000。
将实施例1~3所制得的端羟基超支化聚酯接枝环氧大豆油超分散剂，用于改性聚烯烃（如聚丙烯、聚乙烯或聚氯乙烯等）树脂、木纤维、竹纤维、玻璃纤维、碳酸钙粉体、滑石粉等共混体系制备得到木塑门窗复合材料，不仅能有效改善聚烯烃（如聚丙烯、聚乙烯或聚氯乙烯等）树脂与木纤维、竹纤维、玻璃纤维、碳酸钙粉体、滑石粉等之间的界面相容性，还有利于提高木塑门窗复合材料的力学性能，降低吸水率和收缩膨胀率，而且能改善复合材料的润滑度和表面光洁度。
Claims (2)
1.一种端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法，其特征在于具体步骤为：
(1)在250mL三口烧瓶中加入20~25g环氧大豆油、20~25 g三(羟甲基)氨基甲烷、0.2~0.4g四氟硼酸和100~120g异丙醇，在65~75℃下搅拌反应25~28h后，蒸馏除去异丙醇；反应物用饱和硫酸钠溶液洗涤，除去未完全反应的三(羟甲基)氨基甲烷，干燥后得到粘稠状棕黄色液体，即为大豆油多元醇；
(2)称取80~100mL四氢呋喃和50~80 uL甲醇钾加入步骤(1)制得的大豆油多元醇中，在氮气保护下于50~60℃搅拌1h；然后加入20~30mL二氧六环，升高温度到95℃后，缓慢滴加8~10mL环氧丙醇，继续恒温搅拌反应5~6h，待反应结束后冷至室温，用50~70mL甲醇反复洗涤3次，所得产物置于60℃的真空干燥箱中烘干10h，即制得木塑门窗复合材料用端羟基超支化聚酯接枝环氧大豆油超分散剂，其分子量为2500~3000。
2.一种如权利要求1所述的端羟基超支化聚酯接枝环氧大豆油超分散剂的制备方法，其特征在于该制备方法制得的端羟基超支化聚酯接枝环氧大豆油超分散剂应用于木塑门窗复合材料的填料表面改性，所述填料包括木粉、竹粉、玻璃纤维、碳酸钙和滑石粉。
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