CN106883345A - 一种脲醛树脂改性聚丙烯酰胺有机‑无机复合微球及其制备方法 - Google Patents
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Abstract
本发明公开了一种脲醛树脂改性聚丙烯酰胺有机‑无机复合微球,由以下重量份的原料组成:丙烯酰胺55‑74份,膨润土23‑38份,蒸馏水适量,硫酸镁13‑24份,N,N′‑亚甲基双丙烯酰胺5‑13份,二甲基二烯丙基氯化铵7‑13份,过硫酸铵2‑5份,丙酮适量,甲醛46‑57份,尿素46‑57份,N,N,N',N'‑四甲基乙二胺5‑13份,司盘80 0.8‑3份,环己烷120‑160份,盐酸溶液适量。本发明利用非离子单体丙烯酰胺插层聚合改性膨润土,之后以聚丙烯酰胺‑膨润土微凝胶为骨架与脲醛树脂交联,在微凝胶表面上形成致密的脲醛树脂包覆层,得到具有核‑壳结构的三元复合凝胶微球,具有良好的吸水膨胀、耐盐和热稳定性能。
Description
技术领域
本发明涉及聚丙烯酰胺,具体地说一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球及其制备方法。
背景技术
聚丙烯酰胺及其衍生物是一类用途广泛的水溶性高分子材料,可用作絮凝剂、纸张增强剂和助留助滤剂等,已应用于水处理、造纸和石油开采等领域。交联型聚丙烯酰胺微球由于具有吸水、保水和溶胀等性能,可用作土壤保水剂、油田堵水剂和“尿不湿”等材料。
刘学贵、王恩德、邵红等人在其《新型聚丙烯酰胺改性膨润土防渗材料的研究》一文中,本文以吉林省刘房子天然钠基膨润土为原料,选用聚丙烯酰胺作为改性剂,采用水溶液聚合法,对膨润土进行插层改性,合成了聚丙烯酰胺改性膨润土材料,具有较好的吸水膨胀、耐盐和热稳定性能,研究了改性膨润土防渗材料去除垃圾渗滤液中主要污染物的有效性和控制垃圾渗滤液渗透的可行性。
脲醛树脂泡沫是一种富含各种矿质元素的肥料,如含铵、钠、钙、钾、镁、磷酸盐、硫酸盐、硝酸盐、氯化物、碳酸盐、尿素以及微量元素,能够改善土壤结构。
发明内容
针对现有技术的不足,本发明的目的在于提供一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球及其制备方法,得到粒径均匀的高性能聚合物微球。
一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球,由以下重量份的原料组成:丙烯酰胺55-74份,膨润土23-38份,蒸馏水适量,硫酸镁13-24份,N,N′-亚甲基双丙烯酰胺5-13份,二甲基二烯丙基氯化铵7-13份,过硫酸铵2-5份,丙酮适量,甲醛46-57份,尿素46-57份,N,N,N',N'-四甲基乙二胺5-13份,司盘80 0.8-3份,环己烷120-160份,盐酸溶液适量。
具体步骤如下:
(1)称取膨润土加入到蒸馏水中,搅拌0.5-2小时,使其均匀分散在水溶液中,形成均匀稳定的膨润土悬浮液;
(2)聚丙烯酰胺/膨润土复合微凝胶的制备:
在装有搅拌器和温度控制的反应容器中,称取硫酸镁,溶解到蒸馏水中,待完全溶解后将二分之一份的上述膨润土悬浮液加入到反应器中,再加入反应单体丙烯酰胺、N,N′-亚甲基双丙烯酰胺,并加入二甲基二烯丙基氯化铵、过硫酸铵,分散15-40分钟后,再加入促进剂N,N,N',N'-四甲基乙二胺,之后加入余下的膨润土悬浮液,充分混合均匀,在N2保护下室温聚合反应6-12小时,所得产物经蒸馏水和丙酮多次交替洗涤,洗涤后的产品自然晾干,即得粉末状的聚丙烯酰胺/膨润土复合微凝胶;
(3)含有反应前驱体的微凝胶的制备:将步骤(2)所得微凝胶加入到甲醛与尿素的混合液中,用盐酸溶液调整pH值至2-3,在室温条件下充分溶胀10-15小时;
(4)称取司盘80,加入到含有环己烷的反应瓶中,在N2保护下进行充分乳化,形成油相,室温时,在N2保护条件下将上述含有反应前驱体的微凝胶加入到充分乳化的油相中,充分分散0.5-3小时,将体系温度恒定至45-65℃,反应4-7小时,产品经蒸馏水和丙酮多次交替洗涤后自然晾干,即得。
其中,所述的丙烯酰胺为非离子单体丙烯酰胺。
其中,步骤(3)所述的甲醛与尿素的混合液由甲醛溶液于尿素溶液混合组成,两者体积比1:1。
其中,所述的甲醛溶液和尿素溶液的初始浓度均为1.03mol/L。
与现有技术相比,本发明具有以下优点:
(1)本发明利用非离子单体丙烯酰胺插层聚合改性膨润土,将阳离子聚丙烯酰胺嵌入到膨润土层间,通过范德华力和氢键结合到膨润土层间,层间距扩大,片层结构被破坏,得到了插层型的聚丙烯酰胺/膨润土纳米复合物,其中膨润土主要担负改性膨润上材料的骨架支撑作用。
(2)之后以聚丙烯酰胺-膨润土微凝胶为骨架与脲醛树脂交联,在微凝胶表面上形成致密的脲醛树脂包覆层,得到具有核-壳结构的三元复合凝胶微球,得到的多孔型凝胶微球粒径均匀,产品具有良好的吸水膨胀、耐盐和热稳定性能。
具体实施方式
一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球,由以下重量份的原料组成:丙烯酰胺65份,膨润土33份,蒸馏水适量,硫酸镁21份,N,N′-亚甲基双丙烯酰胺8份,二甲基二烯丙基氯化铵9份,过硫酸铵3份,丙酮适量,甲醛52份,尿素52份,N,N,N',N'-四甲基乙二胺10份,司盘80 2份,环己烷140份,盐酸溶液适量。
具体步骤如下:
(1)称取膨润土加入到蒸馏水中,搅拌2小时,使其均匀分散在水溶液中,形成均匀稳定的膨润土悬浮液;
(2)聚丙烯酰胺/膨润土复合微凝胶的制备:
在装有搅拌器和温度控制的反应容器中,称取硫酸镁,溶解到蒸馏水中,待完全溶解后将二分之一份的上述膨润土悬浮液加入到反应器中,再加入反应单体丙烯酰胺、N,N′-亚甲基双丙烯酰胺,并加入二甲基二烯丙基氯化铵、过硫酸铵,分散35分钟后,再加入促进剂N,N,N',N'-四甲基乙二胺,之后加入余下的膨润土悬浮液,充分混合均匀,在N2保护下室温聚合反应9小时,所得产物经蒸馏水和丙酮多次交替洗涤,洗涤后的产品自然晾干,即得粉末状的聚丙烯酰胺/膨润土复合微凝胶;
(3)含有反应前驱体的微凝胶的制备:将步骤(2)所得微凝胶加入到甲醛与尿素的混合液中,用盐酸溶液调整pH值至2.5,在室温条件下充分溶胀13小时;
(4)称取司盘80,加入到含有环己烷的反应瓶中,在N2保护下进行充分乳化,形成油相,室温时,在N2保护条件下将上述含有反应前驱体的微凝胶加入到充分乳化的油相中,充分分散2小时,将体系温度恒定至55℃,反应6小时,产品经蒸馏水和丙酮多次交替洗涤后自然晾干,即得。
其中,所述的丙烯酰胺为非离子单体丙烯酰胺。
其中,步骤(3)所述的甲醛与尿素的混合液由甲醛溶液于尿素溶液混合组成,两者体积比1:1。
其中,所述的甲醛溶液和尿素溶液的初始浓度均为1.03mol/L。
Claims (5)
1.一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球,其特征在于,由以下重量份的原料组成:丙烯酰胺55-74份,膨润土23-38份,蒸馏水适量,硫酸镁13-24份,N,N′-亚甲基双丙烯酰胺5-13份,二甲基二烯丙基氯化铵7-13份,过硫酸铵2-5份,丙酮适量,甲醛46-57份,尿素46-57份,N,N,N',N'-四甲基乙二胺5-13份,司盘80 0.8-3份,环己烷120-160份,盐酸溶液适量。
2.根据权利要求1所述的一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球的制备方法,其特征在于,具体步骤如下:
(1)称取膨润土加入到蒸馏水中,搅拌0.5-2小时,使其均匀分散在水溶液中,形成均匀稳定的膨润土悬浮液;
(2)聚丙烯酰胺/膨润土复合微凝胶的制备:
在装有搅拌器和温度控制的反应容器中,称取硫酸镁,溶解到蒸馏水中,待完全溶解后将二分之一份的上述膨润土悬浮液加入到反应器中,再加入反应单体丙烯酰胺、N,N′-亚甲基双丙烯酰胺,并加入二甲基二烯丙基氯化铵、过硫酸铵,分散15-40分钟后,再加入促进剂N,N,N',N'-四甲基乙二胺,之后加入余下的膨润土悬浮液,充分混合均匀,在N2保护下室温聚合反应6-12小时,所得产物经蒸馏水和丙酮多次交替洗涤,洗涤后的产品自然晾干,即得粉末状的聚丙烯酰胺/膨润土复合微凝胶;
(3)含有反应前驱体的微凝胶的制备:将步骤(2)所得微凝胶加入到甲醛与尿素的混合液中,用盐酸溶液调整pH值至2-3,在室温条件下充分溶胀10-15小时;
(4)称取司盘80,加入到含有环己烷的反应瓶中,在N2保护下进行充分乳化,形成油相,室温时,在N2保护条件下将上述含有反应前驱体的微凝胶加入到充分乳化的油相中,充分分散0.5-3小时,将体系温度恒定至45-65℃,反应4-7小时,产品经蒸馏水和丙酮多次交替洗涤后自然晾干,即得。
3.根据权利要求1、2所述的一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球的制备方法,其特征在于,所述的丙烯酰胺为非离子单体丙烯酰胺。
4.根据权利要求2所述的一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球的制备方法,其特征在于,步骤(3)所述的甲醛与尿素的混合液由甲醛溶液于尿素溶液混合组成,两者体积比1:1。
5.根据权利要求2、4所述的一种脲醛树脂改性聚丙烯酰胺有机-无机复合微球的制备方法,其特征在于,所述的甲醛溶液和尿素溶液的初始浓度均为1.03mol/L。
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CN110540619A (zh) * | 2019-03-27 | 2019-12-06 | 福建工程学院 | 一种改性脲醛树脂及其制备方法 |
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CN110540619A (zh) * | 2019-03-27 | 2019-12-06 | 福建工程学院 | 一种改性脲醛树脂及其制备方法 |
CN110540619B (zh) * | 2019-03-27 | 2022-05-03 | 福建工程学院 | 一种改性脲醛树脂及其制备方法 |
CN115846396A (zh) * | 2022-12-07 | 2023-03-28 | 江苏绿岩生态技术股份有限公司 | 沙地变草原免养护的环境仿真方法 |
CN115846396B (zh) * | 2022-12-07 | 2023-11-03 | 江苏绿岩生态技术股份有限公司 | 沙地变草原免养护的环境仿真方法 |
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