CN1824682A - 特高分子阳离子聚丙烯酰胺制备方法 - Google Patents
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Abstract
本发明涉及一种特高分子阳离子聚丙烯酰胺制备方法,由丙烯酰胺、(甲基)丙烯酰氧基乙基三甲基氯化铵水溶液共聚合,包括单体精制、纯化,加入多元引发剂、添加剂,经聚合、保温、造粒、干燥、粉碎、筛分等步骤所组成,可制备分子量2300万、溶解速度≤30分钟的特高分子阳离子聚丙烯酰胺,该方法操作方便,适于规模化生产,制得的产品使用效果显著,性能优越,可作为市政工程、油田污水处理,化工、印染、造纸、炼油等行业的污水和废水处理及制作水产养殖业的净水剂等。具有极强的除浊、除色、除臭及消除一些菌害物质的能力,并有降低COD、BOD、SS功能,尤其对高浊度、高污染水体系更为显著,大大减轻了污染物的排放,产生巨大的环境效益和经济效益,具有显著的应用价值。
Description
技术领域:
本发明涉及一种特高分子阳离子聚丙烯酰胺制备方法,属化工技术领域
背景技术:
目前,市售阳离子聚丙烯酰胺其分子量500-1000万,溶解速度1-3小时,残余单体及不溶物含量高。其制备方法以丙烯酰胺与阳离子单体按不同比例混合,一般采用水溶液共聚法,于体系中通入氮气除氧,加入氧化一还原剂(过硫酸盐——亚硫酸钠或硫酸亚铁),也有加入高温阶段起引发作用的水溶性偶氮盐,聚合浓度一般为40%,于30-40℃温度引发聚合,所用工艺设备为箱式或薄片聚合,并进行保温,以降低残余单体含量。所得聚合物凝胶粘度大,分子量不高,而不能进行造粒。物料放于托盘中分层进入烘箱,鼓热风干燥,由于物料静态相互粘结为一体,导致分子量降解严重,因局部受热产品溶解性差,不溶物含量高,存在聚合周期长、干燥能耗高、产量小、产品质量不够稳定。
发明内容:
本发明的目的是提供一种特高分子阳离子聚丙烯酰胺制备方法。
本发明以丙烯酰胺与(甲基)丙烯酰氧基乙基三甲基氯化铵水溶液共聚合法。
本发明采用的丙烯酰胺水溶液单体经D113(大孔弱酸性丙烯酸系树脂)、001×7(强酸性苯乙烯系树脂)、201×7(强碱性苯乙烯系树脂)离子交换树脂精制,(甲基)丙烯酰氧基乙基三甲基氯化铵经醋酸丁酯抽提纯化,以防止单体杂质阻聚及一些杂质在共聚合中产生交联,形成聚合物的不溶或难溶。将丙烯酰胺水溶液与阳离子单体按比例混合均匀,可制备不同阳离子度的产品,采用近似绝热水溶液共聚合工艺,聚合体系中,通入高纯氮(99.999%)除氧。
本发明聚合体系中加入的添加剂有:螯合剂为乙二胺四乙酸二钠,链转移剂为甲酸钠、链增长剂为β-2甲氨基丙腈、链调节剂为乙二胺,按加入共聚单体重量百分比计分别为0.01%-0.25%,0.015%-0.25%,0.15%-2.5%,0.02%-0.5%。
本发明采用过硫酸盐、亚硫酸盐、水溶性有机偶氮盐多元引发剂,过硫酸盐包括过硫酸钾、过硫酸胺,亚硫酸盐包括亚硫酸钠、亚硫酸氢钠,水溶性有机偶氮盐为偶氮脒基丙烷盐酸盐,按加入共聚单体重量百分比计分别为0.005%-0.15%,0.005%-0.15%,0.01%-1%。过硫酸盐引发剂链转移作用强,单独使用,其获得的阳离子聚丙烯酰胺分子量低,水溶性偶氮盐链转移作用弱,能提高共聚物的分子量,但其低温活性差。加入链增长剂、链调节剂、链转移剂,而有效地保持体系的高聚合速率及单体的转化率,促进链增长,抑制分子间的交联,使反应平稳进行,以获得特高分子阳离子聚丙烯酰胺,且溶解速度快,残余单体低。
共聚合单体水溶液浓度控制在25-40%,聚合起始温度10-30℃,聚合时间2-8小时,保温时间1-6小时。
聚合物凝胶的出料、造粒、干燥为生产中的一大难题。对适于水溶液近似绝热聚合工艺的聚合釜内壁采用硅橡胶防粘涂层,聚合保温后,以0.2-0.6mpa压缩空气压出物料,由于聚合物分子量很高,既粘又韧的凝胶呈硬橡胶状,物料经粗造粒,采用特制的聚丙烯酰胺造粒机造粒,造粒后的物料粒径0.2-0.5毫米。
本发明对所得到的特高分子阳离子聚丙烯酰胺胶粒,经高效防粘技术处理,于60-90℃热风下,呈流化态进行热风干燥0.3-3小时,适用的设备有穿流迥转干燥器、振动流化床干燥器。干燥后的物料经粉碎、筛分得特高分子阳离子聚丙烯酰胺产品。其主要技术性能指标:
分子量≥2300万 固含量≥90%
理论阳离子度(mol):30-70% 溶解速度≤30分钟
残余单体≤0.1% 不溶物≤1%
本发明有如下的明显效果和优点:
1、采用的引发体系及添加剂,能获得特高分子、溶解性好的阳离子聚丙烯酰胺胶体。
2、聚合设备内壁采用硅橡胶涂层,凝胶通过0.2-0.6mpa压缩空气可顺利压出。
3、经造粒后的胶粒,采用高效防粘技术处理,进行热风干燥过程中处松散状态,其干燥能力大、速度快、温度适宜、能耗低,干燥过程中分子量降解小,产品溶解性能好。
本发明制备的阳离子聚丙烯酰胺具有如下特点:
1、本发明的特高分子阳离子聚丙烯酰胺溶解速度快(≤30分钟)、残余单体低、不溶物低、阳离子度一般在30-70%之间。
2、经应用试验,具有强烈的吸附架桥及强电荷中和作用,其用量省,仅为普通阳离子高分子絮凝剂的1/2-1/3,所形成的絮体大而坚实,沉降速度快,易于脱水处理,便于操作。
本发明的特高分子阳离子聚丙烯酰胺可作为市政工程、油田污水处理,化工、印染、造纸、炼油等行业的污水和废水处理及制作水产养殖业的净水剂等。具有极强的除浊、除色、除臭及消除一些菌害物质的能力,并有降低COD、BOD、SS功能,尤其对高浊度、高污染水体系更为显著,大大减轻了污染物的排放,产生巨大的环境效益和经济效益,具有显著的应用价值。
具体实施方式
实施例1:
将经离子交换树脂精制后的丙烯酰胺水溶液391kg(浓度26%),与经醋酸酯溶剂抽提后的甲基丙烯酰氧基乙基三甲基氯化铵254kg(浓度为78%),无离子水355kg,加入聚合釜内,调整起始温度18℃,以共聚单体总重量的百分比(下同)依次加入乙二胺四乙酸二钠0.024%、甲酸钠0.024%、β-二甲氨基丙腈0.2%、乙二胺0.12%,通入高纯氮除氧30分钟后,加入过硫酸铵0.01%、亚硫酸氢钠0.01%、2,2’-偶氮(2-脒基丙烷)二盐酸盐0.05%,继续通氮10分钟后,关闭所有阀门,进行聚合反应4小时,当反应不再升温时,进行保温2小时后用0.3mpa压缩空气将胶体压出进行粗造粒、特制的造粒机造粒,得到粒径0.4毫米颗粒胶体,采用高效防粘技术处理,进入流化态热风干燥器内,1小时后经粉碎、筛分,得到的阳离子聚丙烯酰胺,其产品性能指标:分子量2350万、固含量90%、溶解速度28分钟、残余单体<0.1%。
实施例2:
丙烯酰胺水溶液395kg(浓度27%),丙烯酰氧基乙基三甲基氯化铵248kg(浓度为78%),无离子水357kg,加入聚合釜内,添加剂及引发剂加量,工艺过程同实施例1。其产品性能指标:分子量2480万、固含量91%、溶解速度27分钟、残余单体<0.1%。
Claims (5)
1、特高分子阳离子聚丙烯酰胺制备方法,由单体精制、纯化、水溶液共聚合,保温、造粒、干燥、粉碎、筛分等步骤组成。其特征在于以丙烯酰胺与(甲基)丙烯酰氧基乙基三甲基氯化铵按不同比例混合的水溶液,通入高纯氮(99.999%)除氧,采用多元引发剂、添加剂,由近似绝热聚合工艺而制得。
2、根据权利要求1所述的特高分子阳离子聚丙烯酰胺制备方法,其特征是聚合体系中加入的添加剂:螯合剂为乙二胺四乙酸二钠、链转移剂为甲酸钠、链增长剂为β-二甲氨基丙腈、链调节剂为乙二胺,其加入量分别为共聚单体总重量的:0.01%-0.25%、0.015%-0.25%、0.15%-2.5%、0.02%-0.5%。
3、根据权利要求1所述的特高分子阳离子聚丙烯酰胺制备方法,其特征是聚合体系加入的引发剂:过硫酸盐、亚硫酸盐、水溶性有机偶氮盐,其加入量分别为共聚单体总重量的:0.005%-0.15%、0.005%-0.15%、0.01%-1%。
4、根据权利要求1所述的特高分子阳离子聚丙烯酰胺制备方法,其特征在于水溶液共聚合的单体浓度为25-40%,起始温度10-30℃,聚合时间2-8小时,保温时间1-6小时。
5、根据权利要求1所述的特高分子阳离子聚丙烯酰胺制备方法,其特征在于近似绝热聚合的聚合釜采用硅橡胶防粘涂层。
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CN100422227C (zh) * | 2007-02-01 | 2008-10-01 | 江南大学 | 一种阳离子型交联溶胀功能微球的制备方法 |
CN101274793B (zh) * | 2008-01-11 | 2012-07-04 | 朱凡 | 一种多功能聚丙烯酰胺净水剂的合成方法 |
CN103221608A (zh) * | 2010-11-16 | 2013-07-24 | 巴斯夫欧洲公司 | 纤维素纸浆片的生产 |
CN103772606A (zh) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | 一种造纸助留助滤用聚丙烯酰胺的制备方法 |
CN107445272A (zh) * | 2017-07-21 | 2017-12-08 | 扬州科宇化工有限公司 | 一种海水淡化高分子絮凝剂 |
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CN100422227C (zh) * | 2007-02-01 | 2008-10-01 | 江南大学 | 一种阳离子型交联溶胀功能微球的制备方法 |
CN101274793B (zh) * | 2008-01-11 | 2012-07-04 | 朱凡 | 一种多功能聚丙烯酰胺净水剂的合成方法 |
CN103221608A (zh) * | 2010-11-16 | 2013-07-24 | 巴斯夫欧洲公司 | 纤维素纸浆片的生产 |
CN103221608B (zh) * | 2010-11-16 | 2016-02-10 | 巴斯夫欧洲公司 | 纤维素纸浆片的生产 |
CN103772606A (zh) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | 一种造纸助留助滤用聚丙烯酰胺的制备方法 |
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