CN108864981A - 一种耐水防老化拼板胶的制备方法 - Google Patents

一种耐水防老化拼板胶的制备方法 Download PDF

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CN108864981A
CN108864981A CN201810795652.7A CN201810795652A CN108864981A CN 108864981 A CN108864981 A CN 108864981A CN 201810795652 A CN201810795652 A CN 201810795652A CN 108864981 A CN108864981 A CN 108864981A
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刘茂龙
邓博
陈帅
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Foshan Wan Yang Biological Science And Technology Co Ltd
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Abstract

本发明属于胶粘剂制备技术领域,具体涉及一种耐水防老化拼板胶的制备方法。本发明以黄豆提取液中所含卵磷脂作为乳化剂,卵磷脂具有优良的憎水性能,能够在乳胶膜表面形成疏水层,提高乳胶膜的耐水性,大豆提取液中含有大量不饱和脂肪酸,可通过与纤维表面羟基进行酯化,促进乳液与亚麻纤维的相容性,纤维负载于树脂时,使拼板胶膜的柔韧性得到增强,不易发生脆性断裂,本发明添加钛白粉对亚麻纤维增白,同时钛白粉可作为紫外线吸收剂,从而使高分子拼板胶免遭破坏,此外,在氧化亚麻纤维过程中,通过氯化镍与乙二胺四乙酸螯合,可通过分子间的作用消散辐射至平板胶表面的荧光能量,具有广阔的应用前景。

Description

一种耐水防老化拼板胶的制备方法
技术领域
本发明属于胶粘剂制备技术领域,具体涉及一种耐水防老化拼板胶的制备方法。
背景技术
随着经济的发展,人们对木质家具的需求已经逐渐从注重外观上升到注重材质的层面,而实木木材不能直接用于家具制作,必以实木锯材拼板为实木板材用于制作。集成材可充分利用短小料或者小径材拼接而成,不仅保留了天然木材性能优异、材质均匀的特性,还可以拼接成人造板所不能代替的大规格板材,大大提高了木材的利用率,受到国内国际市场的普遍欢迎。由于我国保护生态环境和森林资源,近年来可利用森林、木材资源急剧减少,合理利用现有木材资源尤为重要。
拼板胶是指用于拼接集成材等木制品的粘合剂,适合用于非结构材及结构材用集成材等的拼板粘合。早期实木拼板胶的主要成分为氯丁橡胶、骨胶、牛皮胶、聚胺酯等,一般采用甲苯、二甲苯、二氯甲烷、三氯甲烷作为溶剂,由于这些物质对身体有害,国外已禁止使用。目前,绝大多数木工用拼板胶是由含活性氢的水基聚合物,如聚乙烯醇的水溶液、聚醋酸乙烯酯乳液、丙烯酸乳液等水性乙烯基树脂为主剂乳液,加入多异氰酸酯为固化剂,即构成水性高分子-异氰酸酯胶粘剂API。API因具有优良的粘接性能与断裂韧性,良好的耐水、耐热性能,不易老化,不含甲醛、苯酚等有害物质,且pH值接近中性,对木材无污染,在全球木材加工业中获得了广泛应用。
现有技术中各种各样的拼板胶,仍然存在胶体不稳定、初期固化强度差、耐水性能差,不能进入水中浸泡、抗老化能力较差、遇高低温时易开胶的缺陷。此外,由于乳液形成的胶膜缺乏柔韧性,使得拼版后的竹/木拼板在日光暴晒极端情况下会出现部分端头开裂现象,从而在外力作用下容易导致竹/木拼板脆性断裂。
因此提供一种粘结强度高、耐水性能好、成本低、制备方法简单的拼板胶及其制备方法己成为当务之亟。
发明内容
本发明主要解决的技术问题,针对目前现有技术中拼板胶耐水性能差,由于乳液形成的胶膜缺乏柔韧性,使得拼版后的竹/木拼板在日光暴晒极端情况下强度变差,会出现部分端头开裂现象,从而在外力作用下容易导致竹/木拼板脆性断裂的缺陷,提供了一种耐水防老化拼板胶的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种耐水防老化拼板胶的制备方法,其特征在于具体制备步骤为:
(1)取50~60g玉米淀粉和200~220mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温,启动搅拌器,以250~270r/min的转速搅拌30~40min,再加入180~200mL去离子水,降温,得到稀释糊化淀粉;
(2)向上述三口烧瓶中加入50~55mL硫酸亚铁溶液,搅拌25~30min后,继续加入60~70mL双氧水,用碳酸氢钠溶液调节pH,搅拌2~3h后,得到氧化淀粉液,将氧化淀粉液与600~700mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中离心处理,去除上层液,得到氧化淀粉;
(3)向烧杯中加入200~230mL氢氧化钠溶液和10~15g乙二胺四乙酸,取95~100g亚麻纤维置于烧杯中浸泡18~20h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1500~1700mL蒸馏水中,向蒸馏水中加入10~12mL氯化镍溶液和70~75mL双氧水,常温反应,减压抽滤去除氧化液得到氧化亚麻纤维;
(4)将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温,干燥,按重量份数计,取20~30份氧化淀粉、40~50份氧化亚麻纤维、10~20份环氧大豆油、20~25份钛白粉装入高速分散机中,分散得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温,浸泡,过滤去除滤液得到改性氧化亚麻纤维;
(5)按重量份数计,取800~1000g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡后过滤,分离得到滤液,按重量份数计,取50~60份丙烯酸丁酯、15~20份甲基丙烯酸羟乙酯、30~40份苯乙烯置于烧杯,搅拌15~20min得到混合单体,取0.5~1.0份滤液和90~100份去离子水,在搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌10~15min,得到单体预乳液,另取4~5份滤液和40~50份去离子水加入至四口烧瓶中作为反应底液,取4.5~5.0份过硫酸铵,溶解于25~30份去离子水中,得到引发剂溶液;
(6)将四口烧瓶移入水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度,保温反应后降温至室温,出料得到耐水防老化拼板胶。
步骤(1)所述的水浴加热升温为80~85℃,降温为35~40℃。
步骤(2)所述的硫酸亚铁溶液的质量分数为3%,双氧水质量分数为20%,碳酸氢钠溶液的质量分数为15%,调节pH为6.0~6.4,高速离心转速为3200~3400r/min,离心处理时间为10~15min。
步骤(3)所述的氢氧化钠溶液的质量分数为20%,亚麻纤维长度为4~5mm,氯化镍溶液的质量分数为10%,双氧水的质量分数为30%,常温反应时间为2~4天。
步骤(4)所述的加热升温为80~90℃,干燥时间为7~8h,高速分散转速为4000~4200r/min,分散时间为10~15min,加热升温为50~55℃,浸泡时间为3~4h。步骤(5)所述的捣碎物用无水乙醇浸泡时间为2~3h,搅拌转速为200~300r/min。
步骤(6)所述的水浴锅温度为80~85℃,控制滴加速率为1~3mL/min,升高温度为160~170℃,保温反应时间为2~3h。
本发明的有益效果是:
(1)本发明以黄豆提取液中所含卵磷脂作为乳化剂,由于卵磷脂表面能较低,能够在乳胶膜表面形成疏水层,提高乳胶膜的耐水性,所制备拼板胶乳液的主单体中含有苯乙烯,本发明通过向聚合物中引入了乙烯基,可实现交联聚合以提高拼板胶稳定性,大豆中卵磷脂属于非离子乳化剂,化学稳定性高,大豆提取液中含有大量不饱和脂肪酸,可通过与纤维表面羟基进行酯化,促进乳液与亚麻纤维的相容性,也能够缓解乳液在固化过程中乳化剂被氧化,在本发明的技术方案条件下合成的拼板胶的乳液粒子可接近纳米级,而且粒径分布较窄,水分子难以进入乳液粒子之间缝隙扩散而形成水囊,从而提升拼板胶的粘结性能与防水性能;
(2)本发明中亚麻纤维经氧化后纤维表面较为粗糙,纤维在拼板胶固化树脂中分布较为均匀,具备一定的界面作用力,当负载作用于树脂时,树脂基体能将部分应力传递到模量较高的亚麻纤维上,在受到外力作用下纤维不是直接被破坏,而是先出现拉丝现象然后断裂,消耗了一部分能量,因此使拼板胶膜的柔韧性得到增强,不易发生脆性断裂,另外氧化后的亚麻纤维具有一定长径比,且其粗糙的表面有利于其与固化拼板胶相容性的提高,受到冲击后产生的应力容易分散,不易断裂,从而提高拼板胶强度,本发明在改性亚麻纤维时添加钛白粉对亚麻纤维增白,同时钛白粉可作为紫外线吸收剂,对紫外线有强烈的吸收作用,它能选择性地吸收对高分子有害的紫外线,并将它的能量转变成对高分子无害的振动能或次级辐射荧光释放出来,从而使高分子拼板胶免遭破坏,此外,在氧化亚麻纤维过程中,通过氯化镍与乙二胺四乙酸螯合,镍的螯合物是一类很好的猝灭剂,可通过分子间的作用消散辐射至平板胶表面的荧光能量,具有广阔的应用前景。
具体实施方式
取50~60g玉米淀粉和200~220mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温至80~85℃,启动搅拌器,以250~270r/min的转速搅拌30~40min,再加入180~200mL去离子水,降温至35~40℃,得到稀释糊化淀粉;向上述三口烧瓶中加入50~55mL质量分数为3%硫酸亚铁溶液,搅拌25~30min后,继续加入60~70mL质量分数为20%的双氧水,用质量分数为15%的碳酸氢钠溶液调节pH至6.0~6.4,搅拌2~3h后,得到氧化淀粉液,将氧化淀粉液与600~700mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中以3200~3400r/min的转速离心处理10~15min,去除上层液,得到氧化淀粉;向烧杯中加入200~230mL质量分数为20%的氢氧化钠溶液和10~15g乙二胺四乙酸,取95~100g长度为4~5mm的亚麻纤维置于烧杯中浸泡18~20h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1500~1700mL蒸馏水中,向蒸馏水中加入10~12mL质量分数为10%的氯化镍溶液和70~75mL质量分数为30%的双氧水,常温反应2~4天,减压抽滤去除氧化液得到氧化亚麻纤维;将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温至80~90℃,干燥7~8h,按重量份数计,取20~30份氧化淀粉、40~50份氧化亚麻纤维、10~20份环氧大豆油、20~25份钛白粉装入高速分散机中,以4000~4200r/min的转速分散10~15min得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温至50~55℃,浸泡3~4h,过滤去除滤液得到改性氧化亚麻纤维;按重量份数计,取800~1000g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡2~3h后过滤,分离得到滤液,按重量份数计,取50~60份丙烯酸丁酯、15~20份甲基丙烯酸羟乙酯、30~40份苯乙烯置于烧杯,搅拌15~20min得到混合单体,取0.5~1.0份滤液和90~100份去离子水,在转速为200~300r/min的搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌10~15min,得到单体预乳液,另取4~5份滤液和40~50份去离子水加入至四口烧瓶中作为反应底液,取4.5~5.0份过硫酸铵,溶解于25~30份去离子水中,得到引发剂溶液;将四口烧瓶移入80~85℃的水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,控制滴加速率为1~3mL/min将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度至160~170℃,保温反应2~3h后降温至室温,出料得到耐水防老化拼板胶。
取50g玉米淀粉和200mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温至80℃,启动搅拌器,以250r/min的转速搅拌30min,再加入180mL去离子水,降温至35℃,得到稀释糊化淀粉;向上述三口烧瓶中加入50mL质量分数为3%硫酸亚铁溶液,搅拌25min后,继续加入60mL质量分数为20%的双氧水,用质量分数为15%的碳酸氢钠溶液调节pH至6.0,搅拌2h后,得到氧化淀粉液,将氧化淀粉液与600mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中以3200r/min的转速离心处理10min,去除上层液,得到氧化淀粉;向烧杯中加入200mL质量分数为20%的氢氧化钠溶液和10g乙二胺四乙酸,取95g长度为4mm的亚麻纤维置于烧杯中浸泡18h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1500mL蒸馏水中,向蒸馏水中加入10mL质量分数为10%的氯化镍溶液和70mL质量分数为30%的双氧水,常温反应2天,减压抽滤去除氧化液得到氧化亚麻纤维;将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温至80℃,干燥7h,按重量份数计,取20份氧化淀粉、40份氧化亚麻纤维、10份环氧大豆油、20份钛白粉装入高速分散机中,以4000r/min的转速分散10min得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温至50℃,浸泡3h,过滤去除滤液得到改性氧化亚麻纤维;按重量份数计,取800g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡2h后过滤,分离得到滤液,按重量份数计,取50份丙烯酸丁酯、15份甲基丙烯酸羟乙酯、30份苯乙烯置于烧杯,搅拌15min得到混合单体,取0.5份滤液和90份去离子水,在转速为200r/min的搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌10min,得到单体预乳液,另取4份滤液和40份去离子水加入至四口烧瓶中作为反应底液,取4.5份过硫酸铵,溶解于25份去离子水中,得到引发剂溶液;将四口烧瓶移入80℃的水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,控制滴加速率为1mL/min将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度至160℃,保温反应2h后降温至室温,出料得到耐水防老化拼板胶。
取55g玉米淀粉和210mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温至83℃,启动搅拌器,以260r/min的转速搅拌35min,再加入190mL去离子水,降温至37℃,得到稀释糊化淀粉;向上述三口烧瓶中加入53mL质量分数为3%硫酸亚铁溶液,搅拌27min后,继续加入65mL质量分数为20%的双氧水,用质量分数为15%的碳酸氢钠溶液调节pH至6.2,搅拌2h后,得到氧化淀粉液,将氧化淀粉液与650mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中以3300r/min的转速离心处理13min,去除上层液,得到氧化淀粉;向烧杯中加入220mL质量分数为20%的氢氧化钠溶液和13g乙二胺四乙酸,取97g长度为4mm的亚麻纤维置于烧杯中浸泡19h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1600mL蒸馏水中,向蒸馏水中加入11mL质量分数为10%的氯化镍溶液和73mL质量分数为30%的双氧水,常温反应3天,减压抽滤去除氧化液得到氧化亚麻纤维;将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温至85℃,干燥7h,按重量份数计,取25份氧化淀粉、45份氧化亚麻纤维、11份环氧大豆油、23份钛白粉装入高速分散机中,以4100r/min的转速分散13min得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温至53℃,浸泡3h,过滤去除滤液得到改性氧化亚麻纤维;按重量份数计,取900g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡2h后过滤,分离得到滤液,按重量份数计,取55份丙烯酸丁酯、17份甲基丙烯酸羟乙酯、35份苯乙烯置于烧杯,搅拌17min得到混合单体,取0.7份滤液和95份去离子水,在转速为250r/min的搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌13min,得到单体预乳液,另取4份滤液和45份去离子水加入至四口烧瓶中作为反应底液,取4.7份过硫酸铵,溶解于27份去离子水中,得到引发剂溶液;将四口烧瓶移入83℃的水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,控制滴加速率为2mL/min将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度至165℃,保温反应2h后降温至室温,出料得到耐水防老化拼板胶。
取60g玉米淀粉和220mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温至85℃,启动搅拌器,以270r/min的转速搅拌40min,再加入200mL去离子水,降温至40℃,得到稀释糊化淀粉;向上述三口烧瓶中加入55mL质量分数为3%硫酸亚铁溶液,搅拌30min后,继续加入70mL质量分数为20%的双氧水,用质量分数为15%的碳酸氢钠溶液调节pH至6.4,搅拌3h后,得到氧化淀粉液,将氧化淀粉液与700mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中以3400r/min的转速离心处理15min,去除上层液,得到氧化淀粉;向烧杯中加入230mL质量分数为20%的氢氧化钠溶液和15g乙二胺四乙酸,取100g长度为5mm的亚麻纤维置于烧杯中浸泡20h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1700mL蒸馏水中,向蒸馏水中加入12mL质量分数为10%的氯化镍溶液和75mL质量分数为30%的双氧水,常温反应4天,减压抽滤去除氧化液得到氧化亚麻纤维;将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温至90℃,干燥8h,按重量份数计,取30份氧化淀粉、50份氧化亚麻纤维、20份环氧大豆油、25份钛白粉装入高速分散机中,以4200r/min的转速分散15min得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温至55℃,浸泡4h,过滤去除滤液得到改性氧化亚麻纤维;按重量份数计,取1000g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡3h后过滤,分离得到滤液,按重量份数计,取60份丙烯酸丁酯、20份甲基丙烯酸羟乙酯、40份苯乙烯置于烧杯,搅拌20min得到混合单体,取1.0份滤液和100份去离子水,在转速为300r/min的搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌15min,得到单体预乳液,另取5份滤液和50份去离子水加入至四口烧瓶中作为反应底液,取5.0份过硫酸铵,溶解于30份去离子水中,得到引发剂溶液;将四口烧瓶移入85℃的水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,控制滴加速率为3mL/min将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度至170℃,保温反应3h后降温至室温,出料得到耐水防老化拼板胶。
对比例以北京市某公司生产的拼板胶作为对比例 对本发明制得的耐水防老化拼板胶和对比例中的拼板胶进行检测,检测结果如表1所示:
参照标准JISK6806-2003进行测试。
剪切强度测试参照国标HG/T2727-2010进行测试。
耐水性测试将本发明制得的耐水防老化拼板胶和对比例中的拼板胶在常温下放置3天,再用60℃的温水浸泡3h,室温水中冷却1h,湿态状态下进行检测。
抗热老化性测试将涂覆有本发明制得的耐水防老化拼板胶和对比例拼板胶的竹/木拼板放置室外暴晒10天,暴晒后测试拼板胶胶线开裂率。
表1性能测定结果
根据表1中数据可知,本发明制得的耐水防老化拼板胶,具有很高的粘接强度及优异的耐水性,且稳定性好,完全满足拼板胶贴合工艺要求,具有广阔的使用前景。

Claims (7)

1.一种耐水防老化拼板胶的制备方法,其特征在于具体制备步骤为:
(1)取50~60g玉米淀粉和200~220mL去离子水装入带有搅拌器的三口烧瓶中,水浴加热升温,启动搅拌器,以250~270r/min的转速搅拌30~40min,再加入180~200mL去离子水,降温,得到稀释糊化淀粉;
(2)向上述三口烧瓶中加入50~55mL硫酸亚铁溶液,搅拌25~30min后,继续加入60~70mL双氧水,用碳酸氢钠溶液调节pH,搅拌2~3h后,得到氧化淀粉液,将氧化淀粉液与600~700mL无水乙醇混合,得到氧化淀粉悬浮液,将氧化淀粉悬浮液置于高速离心机中离心处理,去除上层液,得到氧化淀粉;
(3)向烧杯中加入200~230mL氢氧化钠溶液和10~15g乙二胺四乙酸,取95~100g亚麻纤维置于烧杯中浸泡18~20h后取出,得到软化亚麻纤维,用去离子水冲洗软化亚麻纤维直至洗涤液呈中性,将洗涤后的软化亚麻纤维置于1500~1700mL蒸馏水中,向蒸馏水中加入10~12mL氯化镍溶液和70~75mL双氧水,常温反应,减压抽滤去除氧化液得到氧化亚麻纤维;
(4)将氧化淀粉和氧化亚麻纤维置于烘箱中加热升温,干燥,按重量份数计,取20~30份氧化淀粉、40~50份氧化亚麻纤维、10~20份环氧大豆油、20~25份钛白粉装入高速分散机中,分散得到淀粉乳化悬浮液,将氧化亚麻纤维放入淀粉乳化悬浮液中,加热升温,浸泡,过滤去除滤液得到改性氧化亚麻纤维;
(5)按重量份数计,取800~1000g黄豆置于研钵内捣碎,将捣碎物用无水乙醇浸泡后过滤,分离得到滤液,按重量份数计,取50~60份丙烯酸丁酯、15~20份甲基丙烯酸羟乙酯、30~40份苯乙烯置于烧杯,搅拌15~20min得到混合单体,取0.5~1.0份滤液和90~100份去离子水,在搅拌状态下,将烧杯中的混合单体滴加到烧瓶中,滴加结束后,继续搅拌10~15min,得到单体预乳液,另取4~5份滤液和40~50份去离子水加入至四口烧瓶中作为反应底液,取4.5~5.0份过硫酸铵,溶解于25~30份去离子水中,得到引发剂溶液;
(6)将四口烧瓶移入水浴锅中,加入十分之一的单体预乳液和三分之一的引发剂溶液,搅拌反应,待反应出现蓝相后,加入改性氧化亚麻纤维,将剩余单体预乳液滴加完,滴加完后补加剩余引发剂溶液,并升高温度,保温反应后降温至室温,出料得到耐水防老化拼板胶。
2.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(1)所述的水浴加热升温的温度为80~85℃,降温的温度为35~40℃。
3.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(2)所述的硫酸亚铁溶液的质量分数为3%,双氧水质量分数为20%,碳酸氢钠溶液的质量分数为15%,调节pH为6.0~6.4,高速离心转速为3200~3400r/min,离心处理时间为10~15min。
4.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(3)所述的氢氧化钠溶液的质量分数为20%,亚麻纤维长度为4~5mm,氯化镍溶液的质量分数为10%,双氧水的质量分数为30%,常温反应时间为2~4天。
5.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(4)所述的加热升温为80~90℃,干燥时间为7~8h,高速分散转速为4000~4200r/min,分散时间为10~15min,加热升温为50~55℃,浸泡时间为3~4h。
6.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(5)所述的捣碎物用无水乙醇浸泡时间为2~3h,搅拌转速为200~300r/min。
7.根据权利要求1所述的一种耐水防老化拼板胶的制备方法,其特征在于:步骤(6)所述的水浴锅温度为80~85℃,控制滴加速率为1~3mL/min,升高温度为160~170℃,保温反应时间为2~3h。
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