CN107216413B - 一种聚丙烯酰胺反相乳液的合成方法 - Google Patents
一种聚丙烯酰胺反相乳液的合成方法 Download PDFInfo
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Abstract
本发明属于水溶性高分子材料领域，是一种低乳化剂含量的聚丙烯酰胺反相乳液的合成方法。本发明的技术要点为：分两步聚合，第一步用足量的乳化剂和大量的有机溶剂，保证了聚合过程中不会产生凝胶，不会发生由于散热不及时而发生爆聚的现象。第二步聚合是在第一步聚合的基础上少用或不用乳化剂，由于有第一步的种子乳液，聚合过程中不会产生凝胶或破乳。由于已有部分聚合，第二步聚合产生的聚合热大大减少，通过聚合釜夹套冷却水可达到冷凝的要求，同样也不会发生爆聚的现象，保证了安全生产。这种方法可以使聚合反应的乳化剂含量降低而不会破乳，同时生产的安全性增加，降低了生产成本。
Description
技术领域
本发明涉及水溶性高分子材料领域，特别是一种聚丙烯酰胺反相乳液的合成方法。
背景技术
随着聚合技术的发展，聚丙烯酰胺已由最初干粉(胶体)发展成为现在的干粉、反相乳液两种主要产品。八十年代获得工业化生产的聚丙烯酰胺反相乳液产品，其发展速度相当快。
丙烯酰胺反相乳液聚合时，乳液的稳定性对聚合和产品都是十分重要的指标也是该方法的难点。解决此问题的关键是选择适当的乳化剂系统，因为乳化剂在胶乳粒的最外层构成吸附膜，通过吸附膜的阻隔，可防止粒子粘并，以实现乳液稳定。
反相乳液法生产的聚丙烯酰胺胶乳与水溶液聚合法生产的干粉相比，胶乳的溶解速度快，分子量高且分布窄，残余单体少，聚合反应中粘度小，易散热也易控制，宜于大规模生产。
聚丙烯酰胺干粉产品在使用过程中存在着溶解时间长和易受搅拌剪切降解，需配备专门的干粉溶解装置等弊端。聚丙烯酰胺反相乳液已逐步成为聚丙烯酰胺产品的主流，具有溶解速度快和使用方便的特点，但该产品存在着乳化剂含量过高，另外聚合过程由于单体浓度高，聚合热量大，一般聚合釜很难及时散热造成爆聚或凝胶，甚至发生冲料等事故。
发明内容
本发明的目的在于克服现有技术的不足，提供一种能够稳定聚合、乳化剂含量低的聚丙烯酰胺反相乳液的合成方法。
一种聚丙烯酰胺反相乳液的合成方法，其特征是包括如下步骤：
第一步：在装有搅拌器、温度计、冷凝器和气体进出口的容器中，依次加入质量浓度为30-50％的丙烯酰胺水溶液，加入占丙烯酰胺单体质量0-5％的无水乙酸钠，再按所需要的阴离子度加入占丙烯酰胺摩尔量0-50％的2-丙烯酰胺基-2-甲基丙磺酸,用质量浓度为10-50％的氢氧化钠水溶液调节系统的pH值为3-7，再加入占单体总质量20-40％的一定比例的斯盘类乳化剂和辛基酚聚氧乙烯醚乳化剂；开启搅拌，直到反应物混合均匀，然后加入占丙烯酰胺水溶液体积100-200％的有机溶剂，通氮气驱氧，控制温度为5-35℃，搅拌20-40min，化学引发或紫外光照射引发聚合反应，反应结束后得到聚丙烯酰胺反相乳液半成品。
第二步：在另一带有搅拌器的容器中加入质量浓度为30-50％的丙烯酰胺水溶液，加入占丙烯酰胺单体质量0-5％的无水乙酸钠，按所需要的阴离子度加入占丙烯酰胺摩尔量0-50％的2-丙烯酰胺基-2-甲基丙磺酸,用质量浓度为10-50％的氢氧化钠水溶液调节系统的pH值为3-7，本步骤所用的丙烯酰胺和2-丙烯酰胺基-2-甲基丙磺酸的总剂量是第一步总剂量的0.5-2倍，再加入占单体总质量0-10％的辛基酚聚氧乙烯醚乳化剂作为乳化剂。
第三步：在第一步得到的聚丙烯酰胺反相乳液中加入第二步总液体量体积的0-50％的有机溶剂，将第二步得到的溶液缓慢加到上述聚丙烯酰胺反相乳液中，通氮气驱氧，控制温度为5-35℃，搅拌20-40min，化学引发或紫外光照射引发聚合反应，反应结束后得到低乳化剂含量的聚丙烯酰胺反相乳液成品。
主要特征步骤第一步和第二步中，有机溶剂是煤油、液体石蜡、溶剂油或环己烷中的一种。
主要特征步骤第一步中，斯盘类乳化剂是斯盘20、斯盘40、斯盘60、斯盘80或斯盘85中的一种。
主要特征步骤第一步和第二步中，辛基酚聚氧乙烯醚是OP-4、OP-6、OP-8、OP-10、OP-15、OP-20或OP-30中的一种。
本发明采用两步反相乳液聚合法得到聚丙烯酰胺反相乳液产品，第一步用足量的乳化剂和大量的有机溶剂，保证了聚合过程中不会产生凝胶，在工业生产中由于有效聚合量在反应釜中只占正常量的一半，通过聚合釜夹套的冰水完全可以达到冷凝的要求，不会发生由于散热不及时而发生爆聚的现象。第二步聚合是在第一步聚合的基础上少用或不用乳化剂，由于有第一步的种子乳液，聚合过程中不会产生凝胶或破乳。由于已有部分聚合，第二步聚合产生的聚合热大大减少，通过聚合釜夹套的冰水完全可以达到冷凝的要求，同样也不会发生爆聚的现象，保证了安全生产。这种方法可以使反应釜的产量大大提高，生产规模大，同时产品的乳化剂含量低，使生产成本大大降低。
本发明得到的聚丙烯酰胺反相乳液能广泛应用于絮凝、增稠、减阻、凝胶、粘结、阻垢等领域，特别是污水处理和石油开采行业。
具体实施方式
下面给出本发明的二个最佳实施例：
实施例一
第一步：在装有搅拌器、温度计、冷凝器和气体进出口的500ml四口烧瓶中依次加入43wt％的丙烯酰胺水溶液100g，加入2g无水乙酸钠，加入乳化剂脱水山梨醇单月桂酸酯(斯盘60)7.5g和OP-10 2.5g，搅拌10min后，加入环己烷180ml，控制水浴温度25℃搅拌30min，同时通高纯氮气以除去系统中的氧气。加1％的过硫酸铵水溶液0.1ml和5％的亚硫酸氢钠水溶液0.5ml引发，升至最高温度后，保温反应1h，制得非离子聚丙烯酰胺反相乳液半成品。
第二步：在另一带有搅拌器的300ml烧杯中加入质量浓度为43％的丙烯酰胺水溶液100ml，加入2g无水乙酸钠搅拌至溶解，调整温度至25℃。
第三步：在搅拌条件下将第二步得到的溶液加入到第一步得到的聚丙烯酰胺反相乳液中，将第二步得到的溶液缓慢加到上述聚丙烯酰胺反相乳液中，通高纯氮气驱氧，调整温度至30℃，搅拌30min，加1％的过硫酸铵水溶液0.1ml和5％的亚硫酸氢钠水溶液0.5ml引发，升至最高温度后，保温反应1h，制得非离子聚丙烯酰胺反相乳液成品。
实施例二
第一步：在装有搅拌器、温度计、冷凝器和气体进出口的500ml四口烧瓶中依次加入30wt％的丙烯酰胺水溶液100g，加入37.5g 2-丙烯酰胺基-2-甲基丙磺酸，用质量浓度为20％的氢氧化钠水溶液调节系统的pH值为5.0。加入乳化剂脱水山梨醇单月桂酸酯(斯盘40)12g和OP-103.5g，搅拌10min后，加入环己烷200ml，控制水浴温度25℃搅拌30min，同时通高纯氮气以除去系统中的氧气。加入安息香(1mg在0.1ml冰醋酸中)，用250W的高压汞灯照射体系使之引发，待升至最高温度后，保温反应1h，制得阴离子聚丙烯酰胺反相乳液半成品。
第二步：在另一带有搅拌器的300ml烧杯中加入质量浓度为30％的丙烯酰胺水溶液100ml，加入37.5g 2-丙烯酰胺基-2-甲基丙磺酸，用质量浓度为20％的氢氧化钠水溶液调节系统的pH值为5.0，加入乳化剂OP-10 1.0g，搅拌10min，同时调整温度至15℃。
第三步：在搅拌条件下将第二步得到的溶液缓慢加到第一步得到的聚丙烯酰胺反相乳液中，通高纯氮气驱氧，调整温度至30℃，搅拌30min，加入安息香(1mg在0.1ml冰醋酸中)，用250W的高压汞灯照射体系使之引发，待升至最高温度后，保温反应1h，制得阴离子聚丙烯酰胺反相乳液成品。
Claims (2)
1.一种聚丙烯酰胺反相乳液的合成方法，其特征是包括如下步骤：
(1)在装有搅拌器、温度计、冷凝器和气体进出口的容器中，依次加入质量浓度为30-50％的丙烯酰胺水溶液，加入占丙烯酰胺单体质量0-5％的无水乙酸钠，再按所需要的阴离子度加入占丙烯酰胺摩尔量0-50％的2-丙烯酰胺基-2-甲基丙磺酸,用质量浓度为10-50％的氢氧化钠水溶液调节系统的pH值为3-7，再加入占单体总质量20-40％的一定比例的斯盘类乳化剂和辛基酚聚氧乙烯醚(OP)系列乳化剂；开启搅拌，直到反应物混合均匀，然后加入占丙烯酰胺水溶液体积100-150％的有机溶剂，通氮气或二氧化碳驱氧，控制温度为5-35℃，搅拌20-40min，紫外光照射引发聚合反应，反应结束后得到聚丙烯酰胺反相乳液半成品；
(2)在另一带有搅拌器的容器中加入质量浓度为30-50％的丙烯酰胺水溶液，按所需要的阴离子度加入占丙烯酰胺摩尔量0-50％的2-丙烯酰胺基-2-甲基丙磺酸,用质量浓度为10-50％的氢氧化钠水溶液调节系统的pH值为3-7，本步骤所用的丙烯酰胺和2-丙烯酰胺基-2-甲基丙磺酸的总剂量是第一步总剂量的0.5-2倍，再加入占单体总质量0-10％的辛基酚聚氧乙烯醚(OP)系列作为乳化剂；
(3)在步骤(1)得到的聚丙烯酰胺反相乳液中加入步骤(2)总液体量体积0-50％的有机溶剂，将步骤(2)得到的溶液缓慢加到上述聚丙烯酰胺反相乳液中，通氮气或二氧化碳驱氧，控制温度为5-35℃，搅拌20-40min，紫外光照射引发聚合反应，反应结束后得到低乳化剂含量的聚丙烯酰胺反相乳液成品。
2.根据权利要求1所述的一种聚丙烯酰胺反相乳液的合成方法，其特征是步骤(1)和步骤(2)中，有机溶剂是煤油、液体石蜡、溶剂油或环己烷中的一种；斯盘类乳化剂是斯盘20、斯盘40、斯盘60、斯盘80或斯盘85中的一种；辛基酚聚氧乙烯醚(OP)系列是OP-4、OP-6、OP-8、OP-10、OP-15、OP-20或OP-30中的一种。
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| CN104231162A (zh) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | 聚丙烯酰胺反相微乳液及其制备方法 |
| CN104277174A (zh) * | 2013-07-09 | 2015-01-14 | 中国石油化工股份有限公司 | 聚丙烯酰胺纳米微球体系及其制备方法 |
| CN104292384A (zh) * | 2014-09-19 | 2015-01-21 | 中国海洋石油总公司 | 一种阳离子聚丙烯酰胺反相微乳液的制备方法 |
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| CN104231162A (zh) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | 聚丙烯酰胺反相微乳液及其制备方法 |
| CN104277174A (zh) * | 2013-07-09 | 2015-01-14 | 中国石油化工股份有限公司 | 聚丙烯酰胺纳米微球体系及其制备方法 |
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