CN105085858B - 一种生物改性耐高温聚氨酯胶水的制备方法 - Google Patents
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Abstract
本发明涉及一种生物改性耐高温聚氨酯胶水的制备方法，属于高分子材料技术领域。本发明首先将小麦秸秆颗粒与纤维素酶经过处理得秸秆水解葡萄糖溶液，备用；再聚己内酯二元醇与异佛尔酮二异氰酸酯在‑0.02MPa和升温条件下反应，自然冷却至70℃，保温搅拌，待保温搅拌完成后，再将二羟甲基丙酸，秸秆水解葡萄糖溶液和N‑甲基吡咯烷酮，在水浴加热下，搅拌反应和降温，接着将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，进行高速搅拌和自然冷却即可，本发明的有益效果在于：具有耐高温性，在200～250℃下，具有很好的黏附性能，不会脱落；制备步骤简单，所需成本低。
Description
技术领域
本发明涉及一种生物改性耐高温聚氨酯胶水的制备方法，属于高分子材料技术领域。
背景技术
聚氨酯胶水是分子链中含有氨酯基和异氰酸酯基的胶水，由于含有强极性的异氰酸酯和氨基甲酸酯基，具有很高的反应性，能够室温固化，因而对金属、橡胶、玻璃、陶瓷、塑料、木材、织物、皮革等多种材料都有优良的胶粘性能。聚氨酯的主链柔性很好，其最大特点是耐受冲击震动和弯曲疲劳，剥离强度很高，特别是耐低温性能极其优异，在现有的胶水中独占鳌头。聚氨酯胶水工艺简便，室温和加热均能固化，其软硬度可在很大的范围内进行调节，但其耐热性不佳，在高温条件下粘结缝处的胶水易脱落，粘接性差。
发明内容
本发明主要解决的技术问题：针对目前的聚氨酯胶水耐热性差，导致其在高温条件下粘接性差，易剥落的问题，提供了种生物改性耐高温聚氨酯胶水的制备方法，本发明利用制备得的秸秆水解葡萄糖溶液去改性聚氨酯胶水，本发明制得的聚氨酯胶水具有耐高温性，在200～250℃下，具有很好的黏附性能，不会脱落，扩大了聚氨酯胶水的适用范围。
为了解决上述技术问题，本发明所采用的技术方案：
(1)选取经清水冲洗，在60～80℃下烘干2～3h的小麦秸秆，将其切成1～3cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得40～100目的小麦秸秆颗粒；
(2)按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合20～24h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合20～24h，待其搅拌混合完成后，将其置于离心机中离心分离30～45min，取上层清液并升温至120～130℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；
(3)按重量份数计，分别选取55～75份的聚己内酯二元醇，20～35份的异佛尔酮二异氰酸酯和5～10份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至120～130℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应2～3h后，自然冷却至70℃，保温搅拌10～15min；
(4)待保温搅拌完成后，再按重量份数计，分别选取30～65份的二羟甲基丙酸，20～35份的上述步骤(2)制备的秸秆水解葡萄糖溶液和15～35的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应20～40min后，对其降温至40～45℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在3000～4500r/min下高速搅拌30～40min后，自然冷却至20～30℃即可制备得一种生物改性耐高温聚氨酯胶水。
所述的步骤(2)中纤维素酶混合液是由纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液。
本发明的应用：首先将将粘接物表面用砂纸打磨去锈，再用丙酮清洗晾干待用，再用上述制备的耐高温胶水利用滚、涂、刷、喷等各种形式均匀涂抹于被粘结物表面，再在其上加压0.1Mpa，控制固化时间3～4h即可，粘接处在200～250℃下，具有很好的黏附性能，不会脱落。
本发明的有益效果是：
(1)具有耐高温性，在200～250℃下，具有很好的黏附性能，不会脱落；
(2)制备步骤简单，所需成本低。
具体实施方式
首先选取经清水冲洗，在60～80℃下烘干2～3h的小麦秸秆，将其切成1～3cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得40～100目的小麦秸秆颗粒；按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合20～24h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合20～24h，待其搅拌混合完成后，将其置于离心机中离心分离30～45min，取上层清液并升温至120～130℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；再按重量份数计，分别选取55～75份的聚己内酯二元醇，20～35份的异佛尔酮二异氰酸酯和5～10份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至120～130℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应2～3h后，自然冷却至70℃，保温搅拌10～15min；待保温搅拌完成后，再按重量份数计，分别选取30～65份的二羟甲基丙酸，20～35份的秸秆水解葡萄糖溶液和15～35的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应20～40min后，对其降温至40～45℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在3000～4500r/min下高速搅拌30～40min后，自然冷却至20～30℃即可制备得一种生物改性耐高温聚氨酯胶水。其中纤维素酶混合液是由纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液。
实例1
首先选取经清水冲洗，80℃下烘干2～3h的小麦秸秆，将其切成3cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得100目的小麦秸秆颗粒；按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合24h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合24h，待其搅拌混合完成后，将其置于离心机中离心分离45min，取上层清液并升温至130℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；再按重量份数计，分别选取75份的聚己内酯二元醇，20份的异佛尔酮二异氰酸酯和5份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至130℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应3h后，自然冷却至70℃，保温搅拌15min；待保温搅拌完成后，再按重量份数计，分别选取65份的二羟甲基丙酸，20份的秸秆水解葡萄糖溶液和15的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应40min后，对其降温至45℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在4500r/min下高速搅拌40min后，自然冷却至30℃即可制备得一种生物改性耐高温聚氨酯胶水。其中纤维素酶混合液是由纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液，首先将木板表面用砂纸打磨去锈，再用丙酮清洗晾干待用，再用上述制备的耐高温胶水利用滚、涂、刷、喷等各种形式均匀涂抹于被粘木板表面，再在其上加压0.1Mpa，控制固化时间4h即可，粘接处在250℃下，具有很好的黏附性能，不会脱落。
实例2
首先选取经清水冲洗，在60℃下烘干2h的小麦秸秆，将其切成1cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得40目的小麦秸秆颗粒；按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合20h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合20h，待其搅拌混合完成后，将其置于离心机中离心分离30min，取上层清液并升温至120℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；再按重量份数计，分别选取55份的聚己内酯二元醇，35份的异佛尔酮二异氰酸酯和10份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至120℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应2h后，自然冷却至70℃，保温搅拌10min；待保温搅拌完成后，再按重量份数计，分别选取30份的二羟甲基丙酸，35份的秸秆水解葡萄糖溶液和35的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应20min后，对其降温至40℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在3000r/min下高速搅拌30min后，自然冷却至20℃即可制备得一种生物改性耐高温聚氨酯胶水。其中纤维素酶混合液是由纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液，首先将粘接物表面用砂纸打磨去锈，再用丙酮清洗晾干待用，再用上述制备的耐高温胶水利用滚、涂、刷、喷等各种形式均匀涂抹于被粘结物表面，再在其上加压0.1Mpa，控制固化时间4h即可，粘接处在210℃下，具有很好的黏附性能，不会脱落。
实例3
首先选取经清水冲洗，在75℃下烘干2h的小麦秸秆，将其切成2cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得60目的小麦秸秆颗粒；按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合23h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合23h，待其搅拌混合完成后，将其置于离心机中离心分离40min，取上层清液并升温至125℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；再按重量份数计，分别选取60份的聚己内酯二元醇，30份的异佛尔酮二异氰酸酯和10份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至115℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应2h后，自然冷却至70℃，保温搅拌12min；待保温搅拌完成后，再按重量份数计，分别选取50份的二羟甲基丙酸，30份的秸秆水解葡萄糖溶液和20份的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应30min后，对其降温至42℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在4000r/min下高速搅拌35min后，自然冷却至25℃即可制备得一种生物改性耐高温聚氨酯胶水。其中纤维素酶混合液是由纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液，首先将粘接物表面用砂纸打磨去锈，再用丙酮清洗晾干待用，再用上述制备的耐高温胶水利用滚、涂、刷、喷等各种形式均匀涂抹于被粘结物表面，再在其上加压0.1Mpa，控制固化时间3.5h即可，粘接处在200℃下，具有很好的黏附性能，不会脱落。
Claims (2)
1.一种生物改性耐高温聚氨酯胶水的制备方法，其特征在于具体制备步骤为：
(1)选取经清水冲洗，在60～80℃下烘干2～3h的小麦秸秆，将其切成1～3cm的秸秆碎片后，置于高速碾磨机中进行粉碎，再对其过筛，得40～100目的小麦秸秆颗粒；
(2)按固液质量比1:20计，将小麦秸秆颗粒和纤维素酶混合液进行搅拌混合20～24h，搅拌速度为800r/min，使纤维素酶混合液水位没过于秸秆，待其搅拌完成后，对其过滤，取滤液并再次加入上述相同体积的纤维素酶混合液，再次在800r/min速度下搅拌混合20～24h，待其搅拌混合完成后，将其置于离心机中离心分离30～45min，取上层清液并升温至120～130℃进行灭酶处理，得秸秆水解葡萄糖溶液，备用；
(3)按重量份数计，分别选取55～75份的聚己内酯二元醇，20～35份的异佛尔酮二异氰酸酯和5～10份的二月桂酸二丁基锡，置于三口烧瓶中，对其升温至120～130℃，并通入氮气，待排除空气后，再对其抽真空至-0.02MPa，使其反应2～3h后，自然冷却至70℃，保温搅拌10～15min；
(4)待保温搅拌完成后，再按重量份数计，分别选取30～65份的二羟甲基丙酸，20～35份的上述步骤(2)制备的秸秆水解葡萄糖溶液和15～35的N-甲基吡咯烷酮加入到冷却至70℃的三口烧瓶中，并在70℃水浴加热下，搅拌反应20～40min后，对其降温至40～45℃，按聚己内酯二元醇、三乙胺盐酸盐和去离子水按质量比为5:1:10，将三乙胺盐酸盐缓慢加入上述降温后的三口烧瓶中，在3000～4500r/min下高速搅拌30～40min后，自然冷却至20～30℃即可制备得一种生物改性耐高温聚氨酯胶水。
2.根据权利要求1所述的一种生物改性耐高温聚氨酯胶水的制备方法，其特征在于：所述的步骤(2)中纤维素酶混合液是纤维素酶、果胶酶和去离子水按质量比2:1:10搅拌混合形成的混合溶液。
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