CN107497484A - 一种负载催化剂的疏水型聚乙烯醇缓释微球及其制备方法 - Google Patents
一种负载催化剂的疏水型聚乙烯醇缓释微球及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种负载催化剂的疏水型聚乙烯醇缓释微球及其制备方法，其特征在于，向聚乙烯醇中加蒸馏水，溶解得聚乙烯醇溶液；将聚乙烯醇溶液滴加到植物油中，加Span80，乳化反应，滴加交联剂戊二醛，搅拌后，加催化剂盐酸，持续搅拌交联反应后，离心分离沉淀，水洗，丙酮脱水，室温下晾干，得缓释微球；将石蜡水浴加热熔化，加吐温60、司盘60，搅拌均匀，加甲基丙烯酸甲酯、过硫酸钾，乳化反应，过滤得复合乳液防水剂；将钛酸丁酯与无水乙醇混合均匀，搅拌下缓慢加入混合溶液中，持续搅拌，得TiO2溶胶，将其与复合乳液防水剂混合均匀，将缓释微球浸入其中，真空干燥，得负载催化剂的缓释微球。
Description
技术领域
本发明涉及缓释微球领域，具体涉及一种负载催化剂的疏水型聚乙烯醇缓释微球及其制备方法。
背景技术
粉煤灰纤维是粉煤灰通过熔融甩丝成纤工艺生产出来的超细无机矿物纤维，目前国内外对于粉煤灰纤维的研究和生产仍处于起步阶段，大部分研究依然停留在纤维抄纸以及纤维板制备等方面。
王程远在其硕士学位论文《粉煤灰纤维板的制备及防水性能研究》中，采用湿法制板工艺利用粉煤灰纤维制备板材，将粉煤灰纤维通过水利搅拌方法进行松解除渣处理，研究了胶粘剂聚乙烯醇、粉煤灰纤维浆料搅拌分散时间、粉煤灰纤维浓度、添加剂等因素对粉煤灰纤维板力学性能的影响，通过改性粉煤灰纤维、改性胶粘剂以及使用防水涂层来提高粉煤灰纤维板的防水性能。但是存在综合性能、防水性能不足。
发明内容
本发明主要解决的技术问题是提供一种负载催化剂的疏水型聚乙烯醇缓释微球及其制备方法，依照该工艺制备的缓释微球具备良好的缓释性能和疏水性能。
本发明所要解决的技术问题采用以下的技术方案来实现：
一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于，按以下步骤进行：
a. 向40-50重量份聚乙烯醇中1:15-20加入蒸馏水，升温至80-90℃水浴加热搅拌1-2h，完全溶解，得透明聚乙烯醇溶液；
b. 磁力搅拌下，将a中所得聚乙烯醇溶液1:1-2滴加到植物油中，加入0.1-0.2重量份表面活性剂Span80，40-60℃下乳化30-40min，形成均匀乳液体系，滴加1-2重量份交联剂戊二醛，搅拌10-20min后，加入0.2-0.5重量份催化剂盐酸，持续搅拌交联反应1-2h后，离心分离沉淀，水洗3-5次，丙酮脱水2-3次，室温下晾干，得缓释微球；
c. 将6-10重量份石蜡在85-95℃下水浴加热，搅拌熔化，缓慢加2-3重量份吐温60、1-2重量份司盘60，搅拌均匀，1:3-5加蒸馏水，继续恒温搅拌1-2h，加5-8重量份甲基丙烯酸甲酯、0.1-0.2重量份过硫酸钾，在70-80℃搅拌乳化反应3-4h，冷却至室温，用100-200目筛网过滤出料，得复合乳液防水剂；
d. 将5-10重量份钛酸丁酯与无水乙醇3-2:1混合均匀，搅拌下1:2-4缓慢加入混合溶液中，持续搅拌2-3h，得TiO2溶胶，将其与c中物料混合均匀，将b中所得微球浸入其中8-10h，85-95℃真空干燥4-6h，得负载催化剂的缓释微球。
其中，步骤b中所述盐酸浓度为0.5-1mol/L；步骤c中所述乳化反应搅拌速度为1000-1100rpm；步骤d中所述混合溶液为盐酸和去离子水1:30-40混合。
本发明的反应机理及有益效果如下：
采用乳化交联法制备聚乙烯醇(PVA)微球，利用乳化剂将水相与油相混合，形成油包水(W/O)的反应体系，PVA含有大量的羟基，在酸性条件下能与交联剂戊二醛发生缩醛反应，戊二醛加入体系后，会以扩散渗透的方式与PVA溶液混合均匀，在盐酸的催化下，二者发生交联反应，固化成球，以PVA水溶液为水相，以植物油为油相，以Span80为表面活性剂，制备得到PVA缓释微球；以司盘60为乳化剂，以过硫酸钾为引发剂，以甲基丙烯酸甲酯为单体，与石蜡乳液进行乳液聚合，得复合乳液防水剂，可用于改善PVA微球的疏水性和尺寸稳定性；通过溶胶凝胶法制备了TiO2水溶胶，将其与复合乳液防水剂混合均匀，将PVA缓释微球浸入其中，得到负载催化剂的缓释微球。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例
一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于，按以下步骤进行：
a. 向40kg聚乙烯醇中1:15加入蒸馏水，升温至80-90℃水浴加热搅拌2h，完全溶解，得透明聚乙烯醇溶液；
b. 磁力搅拌下，将a中所得聚乙烯醇溶液1:2滴加到植物油中，加入0.2kg表面活性剂Span80，40-60℃下乳化35min，形成均匀乳液体系，滴加1kg交联剂戊二醛，搅拌15min后，加入0.5kg催化剂盐酸，持续搅拌交联反应2h后，离心分离沉淀，水洗3次，丙酮脱水3次，室温下晾干，得缓释微球；
c. 将6kg石蜡在85-95℃下水浴加热，搅拌熔化，缓慢加2kg吐温60、1kg司盘60，搅拌均匀，1:5加蒸馏水，继续恒温搅拌2h，加5kg甲基丙烯酸甲酯、0.1kg过硫酸钾，在70-80℃搅拌乳化反应3h，冷却至室温，用100目筛网过滤出料，得复合乳液防水剂；
d. 将5kg钛酸丁酯与无水乙醇2:1混合均匀，搅拌下1:4缓慢加入混合溶液中，持续搅拌3h，得TiO2溶胶，将其与c中物料混合均匀，将b中所得微球浸入其中10h，85-95℃真空干燥6h，得负载催化剂的缓释微球。
其中，步骤b中所述盐酸浓度为1mol/L；步骤c中所述乳化反应搅拌速度为1100rpm；步骤d中所述混合溶液为盐酸和去离子水1:35混合。
Claims (5)
1.一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于：
向聚乙烯醇中加蒸馏水，溶解得聚乙烯醇溶液；将聚乙烯醇溶液滴加到植物油中，加Span80，乳化反应，滴加交联剂戊二醛，搅拌后，加催化剂盐酸，持续搅拌交联反应后，离心分离沉淀，水洗，丙酮脱水，室温下晾干，得缓释微球；将石蜡水浴加热熔化，加吐温60、司盘60，搅拌均匀，加甲基丙烯酸甲酯、过硫酸钾，乳化反应，过滤得复合乳液防水剂；将钛酸丁酯与无水乙醇混合均匀，搅拌下缓慢加入混合溶液中，持续搅拌，得TiO2溶胶，将其与复合乳液防水剂混合均匀，将缓释微球浸入其中，真空干燥，得负载催化剂的缓释微球。
2.一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于：
a. 向40-50重量份聚乙烯醇中1:15-20加入蒸馏水，升温至80-90℃水浴加热搅拌1-2h，完全溶解，得透明聚乙烯醇溶液；
b. 磁力搅拌下，将a中所得聚乙烯醇溶液1:1-2滴加到植物油中，加入0.1-0.2重量份表面活性剂Span80，40-60℃下乳化30-40min，形成均匀乳液体系，滴加1-2重量份交联剂戊二醛，搅拌10-20min后，加入0.2-0.5重量份催化剂盐酸，持续搅拌交联反应1-2h后，离心分离沉淀，水洗3-5次，丙酮脱水2-3次，室温下晾干，得缓释微球；
c. 将6-10重量份石蜡在85-95℃下水浴加热，搅拌熔化，缓慢加2-3重量份吐温60、1-2重量份司盘60，搅拌均匀，1:3-5加蒸馏水，继续恒温搅拌1-2h，加5-8重量份甲基丙烯酸甲酯、0.1-0.2重量份过硫酸钾，在70-80℃搅拌乳化反应3-4h，冷却至室温，用100-200目筛网过滤出料，得复合乳液防水剂；
d. 将5-10重量份钛酸丁酯与无水乙醇3-2:1混合均匀，搅拌下1:2-4缓慢加入混合溶液中，持续搅拌2-3h，得TiO2溶胶，将其与c中物料混合均匀，将b中所得微球浸入其中8-10h，85-95℃真空干燥4-6h，得负载催化剂的缓释微球。
3.根据权利要求2所述的一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于，步骤b中所述盐酸浓度为0.5-1mol/L。
4.根据权利要求2所述的一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于，步骤c中所述乳化反应搅拌速度为1000-1100rpm。
5.根据权利要求2所述的一种负载催化剂的疏水型聚乙烯醇缓释微球的制备方法，其特征在于，步骤d中所述混合溶液为盐酸和去离子水1:30-40混合。
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