CN105400476B - 一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂及其制备方法 - Google Patents
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂及其制备方法，其由环氧树脂、木质素、氢氧化钠、苯酚、甲醛、4,4’‑二氨基二苯醚、均苯四甲酸二酐、4,4’‑二氨基二苯砜、端羧基丁腈橡胶、聚乙烯醇缩丁醛、正丁醇、有机膨润土、氢化蓖麻油、二亚乙基三胺、邻苯二甲酸二丁酯、氧化石墨烯、海泡石绒、纳米锆酸钙、环氧丙烷丁基醚等原料制成。本发明的粘胶剂中环氧树脂和聚酰亚胺具有一定的互补性，可以提高胶体的粘结度和耐高温性能，添加的木质素经过改性使其内部的活性基团与聚酰胺酸、环氧树脂等材料的基团相互作用，增加粘度，添加的其他助剂可以增强胶体的物理和化学性能。
Description
技术领域
本发明涉及一种胶粘剂，具体地说是涉及一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂及其制备方法。
背景技术
环氧树脂和聚酰亚胺是两类性能优良的树脂。环氧树脂的粘附性能好，可在低温固化，掺和性好，但是它的耐高温性能差。聚酰亚胺的综合性能好，耐高温性能较好，另外，聚酰亚胺的合成路线众多，单体简单，但作为胶粘剂时，有一些缺点：如粘结强度还不够高；可溶性的聚酰亚胺的溶剂难以除去；聚酰亚胺的加工温度太高。可见，环氧树脂和聚酰亚胺的性能具有一定的互补性，用聚酰亚胺对环氧树脂进行改性可以综合两者的优点，得到具有良好机械性能和粘结强度的耐高温环氧胶粘剂。
发明内容
本发明的目的是提供一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂及其制备方法。
为达到上述目的，本发明所采取的技术方案为：
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂，由下列重量份的原料配制而成：环氧树脂70-80、木质素10-12、氢氧化钠4-6、苯酚2-4、甲醛1-2、4,4’-二氨基二苯醚40-50、均苯四甲酸二酐20-24、4,4’-二氨基二苯砜7-9、端羧基丁腈橡胶4-6、聚乙烯醇缩丁醛3-5、正丁醇6-8、有机膨润土 7-9、氢化蓖麻油5-6、二亚乙基三胺7-10、邻苯二甲酸二丁酯4-7、氧化石墨烯5-6、海泡石绒4-7、纳米锆酸钙7-9、环氧丙烷丁基醚5-8、环己酮适量。
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂的制备方法，包括以下步骤：
（1）将一定比例的木质素、氢氧化钠、水加入反应釜中搅拌均匀，加热至100℃恒温反应25-30min，然后降温至50℃后加入苯酚反应30-40min，然后在40min内升温至80-85℃，边升温边加入甲醛，反应一段时间后，冷却出料，得到改性木质素；
（2）将4,4’-二氨基二苯醚置于容器中，然后加入的环己酮中，在冰水浴下开始搅拌，待完全溶解后，分多次向其中加入均苯四甲酸二酐，每次加入时间间隔约为 10-15min，并完全溶解，室温条件下搅拌约 10-12h，然后加入氢化蓖麻油、二亚乙基三胺后进行水浴加热至 60-65℃左右，30-40min后冷却到室温后，得到改性聚酰胺酸，待用；
（3）将聚酰胺酸与环氧树脂按照一定的比例共混，然后加入4,4’-二氨基二苯砜、液体端羧基丁腈橡胶、聚乙烯醇缩丁醛、正丁醇、有机膨润土、邻苯二甲酸二丁酯、氧化石墨烯、海泡石绒、纳米锆酸钙、环氧丙烷丁基醚等原料，在水浴70-72℃下搅拌反应3-4h，即得。
本发明的有益效果：
本发明的粘胶剂中环氧树脂和聚酰亚胺具有一定的互补性，可以提高胶体的粘结度和耐高温性能，添加的木质素经过改性使其内部的活性基团与聚酰胺酸、环氧树脂等材料的基团相互作用，增加粘度，添加的其他助剂可以增强胶体的物理和化学性能。
具体实施方式
下面结合具体实施例对本发明所述技术方案作进一步的说明。
实施例1：
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂，由下列重量份（kg）的原料配制而成：环氧树脂70、木质素10、氢氧化钠4、苯酚2、甲醛1、4,4’-二氨基二苯醚40、均苯四甲酸二酐20、4,4’-二氨基二苯砜7、端羧基丁腈橡胶4、聚乙烯醇缩丁醛3、正丁醇6、有机膨润土7、氢化蓖麻油5、二亚乙基三胺7、邻苯二甲酸二丁酯4、氧化石墨烯5、海泡石绒4、纳米锆酸钙7、环氧丙烷丁基醚5、环己酮适量。
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂的制备方法，包括以下步骤：
（1）将一定比例的木质素、氢氧化钠、水加入反应釜中搅拌均匀，加热至100℃恒温反应25-30min，然后降温至50℃后加入苯酚反应30-40min，然后在40min内升温至80-85℃，边升温边加入甲醛，反应一段时间后，冷却出料，得到改性木质素；
（2）将4,4’-二氨基二苯醚置于容器中，然后加入的环己酮中，在冰水浴下开始搅拌，待完全溶解后，分多次向其中加入均苯四甲酸二酐，每次加入时间间隔约为 10-15min，并完全溶解，室温条件下搅拌约 10-12h，然后加入氢化蓖麻油、二亚乙基三胺后进行水浴加热至 60-65℃左右，30-40min后冷却到室温后，得到改性聚酰胺酸，待用；
（3）将聚酰胺酸与环氧树脂按照一定的比例共混，然后加入4,4’-二氨基二苯砜、液体端羧基丁腈橡胶、聚乙烯醇缩丁醛、正丁醇、有机膨润土、邻苯二甲酸二丁酯、氧化石墨烯、海泡石绒、纳米锆酸钙、环氧丙烷丁基醚等原料，在水浴70-72℃下搅拌反应3-4h，即得。
实施例2：
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂，由下列重量份（kg）的原料配制而成：环氧树脂75、木质素11、氢氧化钠5、苯酚3、甲醛1.5、4,4’-二氨基二苯醚45、均苯四甲酸二酐22、4,4’-二氨基二苯砜8、端羧基丁腈橡胶5、聚乙烯醇缩丁醛4、正丁醇7、有机膨润土 8、氢化蓖麻油5.5、二亚乙基三胺8.5、邻苯二甲酸二丁酯5.5、氧化石墨烯5.5、海泡石绒6、纳米锆酸钙8、环氧丙烷丁基醚6.5、环己酮适量。
制备方法同实施例1。
实施例3：
一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂，由下列重量份（kg）的原料配制而成：环氧树脂80、木质素12、氢氧化钠6、苯酚4、甲醛2、4,4’-二氨基二苯醚50、均苯四甲酸二酐24、4,4’-二氨基二苯砜9、端羧基丁腈橡胶6、聚乙烯醇缩丁醛5、正丁醇8、有机膨润土9、氢化蓖麻油6、二亚乙基三胺10、邻苯二甲酸二丁酯7、氧化石墨烯6、海泡石绒7、纳米锆酸钙9、环氧丙烷丁基醚8、环己酮适量。
制备方法同实施例1。
上述实施例1-3制得的改性木质素聚酰胺酸/环氧树脂复合胶粘剂的性能检测结果如下表所示：
表1 实施例1-3制得的改性木质素聚酰胺酸/环氧树脂复合胶粘剂的性能检测结果
| 实施例1 | 实施例2 | 实施例3 | |
| 粘度，mpa.s | 78957 | 86428 | 79648 |
| 拉伸剪切强度，Mpa | 3.62 | 3.44 | 3.25 |
| 拉伸强度，Mpa | 34.5 | 33.2 | 28.4 |
| 剪切强度，Mpa | 17.5 | 21.2 | 18.6 |
| 浸水后拉伸剪切强度（25℃,24h），Mpa | 2.16 | 2.24 | 2.48 |
Claims (1)
1.一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂，其特征在于，由下列重量份的原料配制而成：环氧树脂70-80、木质素10-12、氢氧化钠4-6、苯酚2-4、甲醛1-2、4,4’-二氨基二苯醚40-50、均苯四甲酸二酐20-24、4,4’-二氨基二苯砜7-9、端羧基丁腈橡胶4-6、聚乙烯醇缩丁醛3-5、正丁醇6-8、有机膨润土7-9、氢化蓖麻油5-6、二亚乙基三胺7-10、邻苯二甲酸二丁酯4-7、氧化石墨烯5-6、海泡石绒4-7、纳米锆酸钙7-9、环氧丙烷丁基醚5-8、环己酮适量；
以上所述的一种改性木质素聚酰胺酸/环氧树脂复合胶粘剂的制备方法，包括以下步骤：
(1)将一定比例的木质素、氢氧化钠、水加入反应釜中搅拌均匀，加热至100℃恒温反应25-30min，然后降温至50℃后加入苯酚反应30-40min，然后在40min内升温至80-85℃，边升温边加入甲醛，反应一段时间后，冷却出料，得到改性木质素；
(2)将4,4’-二氨基二苯醚置于容器中，然后加入的环己酮中，在冰水浴下开始搅拌，待完全溶解后，分多次向其中加入均苯四甲酸二酐，每次加入时间间隔为10-15min，并完全溶解，室温条件下搅拌10-12h，然后加入氢化蓖麻油、二亚乙基三胺后进行水浴加热至60-65℃，30-40min后冷却到室温后，得到改性聚酰胺酸，待用；
(3)将改性聚酰胺酸与环氧树脂按照一定的比例共混，然后加入4,4’-二氨基二苯砜、端羧基丁腈橡胶、聚乙烯醇缩丁醛、正丁醇、有机膨润土、邻苯二甲酸二丁酯、氧化石墨烯、海泡石绒、纳米锆酸钙、环氧丙烷丁基醚、改性木质素，在水浴70-72℃下搅拌反应3-4h，即得。
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| EP0388095B1 (en) * | 1989-03-16 | 1996-06-05 | AT&T Corp. | Method of curing polymeric or oligomeric material |
| CN1550523A (zh) * | 2003-05-06 | 2004-12-01 | 藤炭素株式会社 | 生物质树脂组合物、其制法和该生物质树脂组合物成型材料 |
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