CN106497293A - 二氧化硅、聚丙烯酸酯复合乳液的制备方法 - Google Patents
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Abstract
本发明二氧化硅、聚丙烯酸酯复合乳液的制备方法涉及聚氨酯工业领域,具体涉及二氧化硅、聚丙烯酸酯复合乳液的制备方法,包括以下步骤:硅溶胶的制备将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25‑30wt%的硅溶胶;半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液,将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N‑丙烯酸丁酯分别加入装有机械搅拌器;本发明操作简单,方便加工,且随复合乳液膜的拉伸强度和断裂伸长率都有所提升,而吸水率下降,提升了复合乳液膜的热稳定性能。
Description
技术领域
本发明涉及聚氨酯工业领域,具体涉及二氧化硅、聚丙烯酸酯复合乳液的制备方法。
背景技术
聚丙烯酸酯乳液材料具有很多优异的性能,如价格低廉、可塑性强,几乎没有挥发性气体(VOC)以及优异的耐候性等,但其疏水性能不好、抗水性能较弱、力学性能一般、耐热性能不佳等缺点限制了其更广泛的应用。因此,提高聚丙烯酸酯材料的疏水性能、力学性能和热性能成为该领域的研究热点。
将聚丙烯酸酯乳液与纳米无机粒子复合,利用纳米无机粒子的特殊性质可改善聚丙烯酸酯乳液成膜后的机械性能和热性能,其中,将纳米二氧化硅,加入到聚丙烯酸酯乳液是一种有效的改性方法。然而,纳米二氧化硅与丙烯酸酯乳液直接混合时分散难度较大,容易絮凝甚至沉淀,常用的改进方法是利用硅烷偶联剂来预处理纳米二氧化硅,但成本较高,且纳米二氧化硅团聚的问题依然存在。
研究发现,硅溶胶可以较容易和聚合物形成有机/无机复合材料,且可达到较高的含量。应用于复合乳液领域的硅溶胶一般利用正硅酸乙酯(TEOS)来制备,采用成本更低、水解速度更快的正硅酸甲酯(TMOs)制备硅溶胶并用于复合材料领域的报道却很少。
发明内容
本发明目的在于提供一种操作简单,方便加工,且随复合乳液膜的拉伸强度和断裂伸长率都有所提升,而吸水率下降,提升了复合乳液膜的热稳定性能的二氧化硅、聚丙烯酸酯复合乳液的制备方法。
本发明二氧化硅、聚丙烯酸酯复合乳液的制备方法,包括以下步骤:
第一步,硅溶胶的制备
将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25-30wt%的硅溶胶;
第二步,半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液
将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N-丙烯酸丁酯分别加入装有机械搅拌器、温度计和回流冷凝器的500mL四口烧瓶中,常温下搅拌1h,升温至70-75度,加入溶有0.32g过硫酸铵水溶液,继续搅拌反应0.5h,在随后的2 h内滴加完129甲基丙烯酸甲酯和12gN-丙烯酸丁酯混合液,继续保温反应1 h后自然冷却至室温后过滤得到复合乳液。
优选地,1:1的氢氧化铵溶液的体积为5mL,与1:1的氢氧化铵溶液混合的水的体积为60mL。
优选地,第二步中搅拌的速度为400转/min。
本发明操作简单,方便加工,且随复合乳液膜的拉伸强度和断裂伸长率都有所提升,而吸水率下降,提升了复合乳液膜的热稳定性能。
具体实施方式
实施例一:
本发明二氧化硅、聚丙烯酸酯复合乳液的制备方法,包括以下步骤:
第一步,硅溶胶的制备
将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25-30wt%的硅溶胶;
第二步,半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液
将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N-丙烯酸丁酯分别加入装有机械搅拌器、温度计和回流冷凝器的500mL四口烧瓶中,常温下搅拌1h,升温至70-75度,加入溶有0.32g过硫酸铵水溶液,继续搅拌反应0.5h,在随后的2 h内滴加完129甲基丙烯酸甲酯和12gN-丙烯酸丁酯混合液,继续保温反应1 h后自然冷却至室温后过滤得到复合乳液。
实施例二:
本发明二氧化硅、聚丙烯酸酯复合乳液的制备方法,包括以下步骤:
第一步,硅溶胶的制备
将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25-30wt%的硅溶胶;
第二步,半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液
将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N-丙烯酸丁酯分别加入装有机械搅拌器、温度计和回流冷凝器的500mL四口烧瓶中,常温下搅拌1h,升温至70-75度,加入溶有0.32g过硫酸铵水溶液,继续搅拌反应0.5h,在随后的2 h内滴加完129甲基丙烯酸甲酯和12gN-丙烯酸丁酯混合液,继续保温反应1 h后自然冷却至室温后过滤得到复合乳液。
1:1的氢氧化铵溶液的体积为5mL,与1:1的氢氧化铵溶液混合的水的体积为60mL。
实施例三:
本发明二氧化硅、聚丙烯酸酯复合乳液的制备方法,包括以下步骤:
第一步,硅溶胶的制备
将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25-30wt%的硅溶胶;
第二步,半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液
将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N-丙烯酸丁酯分别加入装有机械搅拌器、温度计和回流冷凝器的500mL四口烧瓶中,常温下搅拌1h,升温至70-75度,加入溶有0.32g过硫酸铵水溶液,继续搅拌反应0.5h,在随后的2 h内滴加完129甲基丙烯酸甲酯和12gN-丙烯酸丁酯混合液,继续保温反应1 h后自然冷却至室温后过滤得到复合乳液。
1:1的氢氧化铵溶液的体积为5mL,与1:1的氢氧化铵溶液混合的水的体积为60mL。
第二步中搅拌的速度为400转/min。
本发明操作简单,方便加工,且随复合乳液膜的拉伸强度和断裂伸长率都有所提升,而吸水率下降,提升了复合乳液膜的热稳定性能。
Claims (3)
1.一种二氧化硅、聚丙烯酸酯复合乳液的制备方法,其特征在于,包括以下步骤:
第一步,硅溶胶的制备
将100mL的正硅酸甲酯加入到三口烧瓶,室温搅拌下将1:1的氢氧化铵溶液与水混合后,经3h缓慢滴加进烧瓶内,持续搅拌3h,获得固含量为30%的甲醇硅溶胶,再经过蒸馏水交换出甲醇,获得固含量为25-30wt%的硅溶胶;
第二步,半连续原位乳液聚合法制备二氧化硅、聚丙烯酸酯复合乳液
将十二烷基苯磺酸钠、烷基酚聚十氧乙烯醚、硅溶胶、200mL去离子水、8 g甲基丙烯酸甲酯和8g N-丙烯酸丁酯分别加入装有机械搅拌器、温度计和回流冷凝器的500mL四口烧瓶中,常温下搅拌1h,升温至70-75度,加入溶有0.32g过硫酸铵水溶液,继续搅拌反应0.5h,在随后的2 h内滴加完129甲基丙烯酸甲酯和12gN-丙烯酸丁酯混合液,继续保温反应1 h后自然冷却至室温后过滤得到复合乳液。
2.如权利要求1所述二氧化硅、聚丙烯酸酯复合乳液的制备方法,其特征在于,1:1的氢氧化铵溶液的体积为5mL,与1:1的氢氧化铵溶液混合的水的体积为60mL。
3.如权利要求2所述二氧化硅、聚丙烯酸酯复合乳液的制备方法,其特征在于,所述第二步中搅拌的速度为400转/min。
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CN106957383A (zh) * | 2017-04-20 | 2017-07-18 | 上海东升新材料有限公司 | 一种土工格栅用苯丙胶乳及其制备方法 |
CN106977662A (zh) * | 2017-04-20 | 2017-07-25 | 上海东升新材料有限公司 | 一种土工格栅用苯丙乳液及其制备方法 |
CN107011475A (zh) * | 2017-04-20 | 2017-08-04 | 上海东升新材料有限公司 | 一种土工格栅用胶乳及其制备方法 |
CN107474180A (zh) * | 2017-09-06 | 2017-12-15 | 张永霞 | 一种二氧化硅聚酯乳液的制备方法 |
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CN106916246A (zh) * | 2017-04-20 | 2017-07-04 | 上海东升新材料有限公司 | 一种用于土工格栅的乳液及制备方法 |
CN106957383A (zh) * | 2017-04-20 | 2017-07-18 | 上海东升新材料有限公司 | 一种土工格栅用苯丙胶乳及其制备方法 |
CN106977662A (zh) * | 2017-04-20 | 2017-07-25 | 上海东升新材料有限公司 | 一种土工格栅用苯丙乳液及其制备方法 |
CN107011475A (zh) * | 2017-04-20 | 2017-08-04 | 上海东升新材料有限公司 | 一种土工格栅用胶乳及其制备方法 |
CN107474180A (zh) * | 2017-09-06 | 2017-12-15 | 张永霞 | 一种二氧化硅聚酯乳液的制备方法 |
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