CN106009030B - 一种大尺寸聚丙烯酰胺晶胶的制备方法 - Google Patents
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Abstract
本发明涉及一种大尺寸聚丙烯酰胺晶胶的制备方法,属于晶胶制备技术领域。本发明通过将荞麦淀粉改性制备颗粒荞麦淀粉,与水结合后体积膨胀,作为聚合晶胶基质骨架,随后聚合制备聚丙烯酰胺晶胶,再在37℃下,由于超细荞麦颗粒尺寸均一,通过淀粉酶使淀粉骨架水解形成均一孔隙,本发制备的大尺寸聚丙烯酰胺晶胶直径为145~200mm,厚度为22~23mm,较同类晶胶介质尺寸提高15~20,同时晶胶介质孔隙率可达81~82%,且通过淀粉资源化制备,节约资源,绿色环保无污染。
Description
技术领域
本发明涉及一种大尺寸聚丙烯酰胺晶胶的制备方法,属于晶胶制备技术领域。
背景技术
与传统凝胶相比,晶胶的显著特征是具有相互连通的超大孔隙;与一般大孔材料相比,晶胶具有良好的弹性,在承受较强的压力时,晶胶材料会被压缩,压力消失后,其形状会复原;即使其体积被压缩为原来的50%,其内部的孔结构也不会受到明显破坏。晶胶材料可以干燥并储存,再次使用时方便简单,只需将材料浸入相应的液相中,即可快速复原,一般膨胀过程仅需数秒。晶胶基质在低温下由溶剂结晶和单体聚合而形成。基质单体要满足在所用溶剂中具有很好的溶解性,在溶剂结晶条件下不凝固,在低温条件下可发生适当速度的聚合反应等要求。
丙烯酞胺作为介质的制备材料一直很受欢迎,它也是常用的电泳凝胶材料。这是因为聚丙烯酞胺具有亲水性好、pH值稳定、不易生物降解、有一定的机械强度等特点,在低温下可以缓慢聚合,是较好的生物相容性聚合物。从制备所得的晶胶性能来看,聚丙烯酞胺基晶胶具有弹性好、孔隙大、连通性好以及吸水复原能力强等优点,因此在晶胶层析分离研究中应用较多。但是目前制备的晶胶体积都很小,对生物料液的处理量远远未能达到工业生产水平,但是普通通过整体介质放大制备大尺寸晶胶时,聚合反应发生时反应热均匀释放不均匀,造成整体介
质的孔隙不均,性能下降等问题,所以制备一种稳定的大尺寸聚丙烯酰胺晶胶很有必要。
发明内容
本发明所要解决的技术问题:针对目前制备的晶胶体积小,对生物料液的处理量远远未能达到工业生产水平,而通过整体介质放大制备大尺寸晶胶时,聚合反应发生时反应热均匀释放不均匀,造成整体介质的孔隙不均,性能下降的问题,提供了一种通过将荞麦淀粉改性制备颗粒荞麦淀粉,随后在冷水下,与水结合后体积膨胀,作为聚合晶胶基质骨架,随后聚合制备聚丙烯酰胺晶胶,再在37℃下,通过淀粉酶使淀粉骨架水解,由于超细荞麦颗粒尺寸均一,待水解完成后,形成均一孔隙,有效的解决了现有晶胶体积小,而放大晶胶时造成整体介质的孔隙不均,性能下降的问题。
为解决上述技术问题,本发明采用如下所述的技术方案是:
(1)收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工8~10h后并过筛,制备得150~160目超细荞麦淀粉,随后按重量份数计,分别称量25~30份超细荞麦淀粉、45~55份1mol/L氢氧化钠溶液和45~50份无水乙醇置于三口烧瓶中,在65~80℃下水浴加热1~2h,控制搅拌速度为350~400r/min;
(2)待水浴加热完成后,抽滤并收集滤饼,在0~5℃下用去离子水洗涤3~5次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在200~300W下超声分散处理10~15min,制备得淀粉颗粒悬浮液;
(3)按重量份数计,分别称量25~30份聚丙烯单体、45~50份上述制备的淀粉颗粒悬浮液、5~10份N,N’-亚甲基双丙烯酰胺和2~3份过硫酸铵置于三口烧瓶中,在55~60℃下水浴加热35~40min;
(4)待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应25~30min;
(5)待保温加热完成后,再按2℃/min缓慢降温,待温度将至0~5℃后,停止降温并保温反应10~12h,待保温反应完成后,将其置于室温下静置1~2h,过滤并收集滤饼,用去离子水洗涤2~3次,随后真空冷冻干燥3~5h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
本发明的应用方法是:将上述制备的大尺寸聚丙烯酰胺晶胶逐块装填在内径140mm,高度为150mm的层析装置内,随后对其加水并使其在1分钟内迅速膨胀,紧紧贴壁并相互压紧,以保证柱效,制备得层析柱。
本发明与其他方法相比,有益技术效果是:
(1)本发制备的大尺寸聚丙烯酰胺晶胶直径为145~200mm,厚度为22~23mm,较同类晶胶介质尺寸提高15~20%,同时晶胶介质孔隙率可达81~82%;
(2)通过淀粉资源化制备,节约资源,绿色环保无污染。
具体实施方式
首先收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工8~10h后并过筛,制备得150~160目超细荞麦淀粉,随后按重量份数计,分别称量25~30份超细荞麦淀粉、45~55份1mol/L氢氧化钠溶液和45~50份无水乙醇置于三口烧瓶中,在65~80℃下水浴加热1~2h,控制搅拌速度为350~400r/min;待水浴加热完成后,抽滤并收集滤饼,在0~5℃下用去离子水洗涤3~5次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在200~300W下超声分散处理10~15min,制备得淀粉颗粒悬浮液;按重量份数计,分别称量25~30份聚丙烯单体、45~50份上述制备的淀粉颗粒悬浮液、5~10份N,N’-亚甲基双丙烯酰胺和2~3份过硫酸铵置于三口烧瓶中,在55~60℃下水浴加热35~40min;待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应25~30min;待保温加热完成后,再按2℃/min缓慢降温,待温度将至0~5℃后,停止降温并保温反应10~12h,待保温反应完成后,将其置于室温下静置1~2h,过滤并收集滤饼,用去离子水洗涤2~3次,随后真空冷冻干燥3~5h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
实例1
首先收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工8h后并过筛,制备得150目超细荞麦淀粉,随后按重量份数计,分别称量25份超细荞麦淀粉、45份1mol/L氢氧化钠溶液和45份无水乙醇置于三口烧瓶中,在65℃下水浴加热1h,控制搅拌速度为350r/min;待水浴加热完成后,抽滤并收集滤饼,在0℃下用去离子水洗涤3次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在200W下超声分散处理10min,制备得淀粉颗粒悬浮液;按重量份数计,分别称量25份聚丙烯单体、45份上述制备的淀粉颗粒悬浮液、5份N,N’-亚甲基双丙烯酰胺和2份过硫酸铵置于三口烧瓶中,在55℃下水浴加热35min;待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应25min;待保温加热完成后,再按2℃/min缓慢降温,待温度将至0℃后,停止降温并保温反应10h,待保温反应完成后,将其置于室温下静置1h,过滤并收集滤饼,用去离子水洗涤2次,随后真空冷冻干燥3h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
实例2
首先收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工9h后并过筛,制备得155目超细荞麦淀粉,随后按重量份数计,分别称量27份超细荞麦淀粉、47份1mol/L氢氧化钠溶液和47份无水乙醇置于三口烧瓶中,在70℃下水浴加热1h,控制搅拌速度为370r/min;待水浴加热完成后,抽滤并收集滤饼,在2℃下用去离子水洗涤4次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在250W下超声分散处理12min,制备得淀粉颗粒悬浮液;按重量份数计,分别称量27份聚丙烯单体、47份上述制备的淀粉颗粒悬浮液、7份N,N’-亚甲基双丙烯酰胺和3份过硫酸铵置于三口烧瓶中,在57℃下水浴加热37min;待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应27min;待保温加热完成后,再按2℃/min缓慢降温,待温度将至2℃后,停止降温并保温反应11h,待保温反应完成后,将其置于室温下静置2h,过滤并收集滤饼,用去离子水洗涤3次,随后真空冷冻干燥4h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
实例3
首先收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工10h后并过筛,制备得160目超细荞麦淀粉,随后按重量份数计,分别称量30份超细荞麦淀粉、55份1mol/L氢氧化钠溶液和50份无水乙醇置于三口烧瓶中,在80℃下水浴加热2h,控制搅拌速度为400r/min;待水浴加热完成后,抽滤并收集滤饼,在5℃下用去离子水洗涤5次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在300W下超声分散处理15min,制备得淀粉颗粒悬浮液;按重量份数计,分别称量30份聚丙烯单体、50份上述制备的淀粉颗粒悬浮液、10份N,N’-亚甲基双丙烯酰胺和3份过硫酸铵置于三口烧瓶中,在60℃下水浴加热40min;待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应30min;待保温加热完成后,再按2℃/min缓慢降温,待温度将至5℃后,停止降温并保温反应12h,待保温反应完成后,将其置于室温下静置2h,过滤并收集滤饼,用去离子水洗涤3次,随后真空冷冻干燥5h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
Claims (1)
1.一种大尺寸聚丙烯酰胺晶胶的制备方法,其特征在于具体制备步骤为;
(1)收集干燥荞麦淀粉,将其置于高能纳米冲击磨中,按磨介与荞麦淀粉体积比2:1,加工8~10h后并过筛,制备得150~160目超细荞麦淀粉,随后按重量份数计,分别称量25~30份超细荞麦淀粉、45~55份1mol/L氢氧化钠溶液和45~50份无水乙醇置于三口烧瓶中,在65~80℃下水浴加热1~2h,控制搅拌速度为350~400r/min;
(2)待水浴加热完成后,抽滤并收集滤饼,在0~5℃下用去离子水洗涤3~5次,制备得荞麦淀粉颗粒,按质量比1:5,将荞麦淀粉颗粒与50℃去离子水搅拌混合,在200~300W下超声分散处理10~15min,制备得淀粉颗粒悬浮液;
(3)按重量份数计,分别称量25~30份聚丙烯单体、45~50份上述制备的淀粉颗粒悬浮液、5~10份N,N’-亚甲基双丙烯酰胺和2~3份过硫酸铵置于三口烧瓶中,在55~60℃下水浴加热35~40min;
(4)待加热完成后,按1℃/min速度缓慢降温,待温度降至37℃时,停止降温,保温加热并对三口烧瓶滴加质量浓度1%唾液淀粉酶水溶液,控制滴加量为淀粉颗粒悬浮液质量5%,待滴加完成后,保温反应25~30min;
(5)待保温加热完成后,再按2℃/min缓慢降温,待温度将至0~5℃后,停止降温并保温反应10~12h,待保温反应完成后,将其置于室温下静置1~2h,过滤并收集滤饼,用去离子水洗涤2~3次,随后真空冷冻干燥3~5h,即可制备得一种大尺寸聚丙烯酰胺晶胶。
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