CN107011529A - 一种纳米纤维增强的超顺磁性聚乙烯醇复合膜及其制备方法 - Google Patents
一种纳米纤维增强的超顺磁性聚乙烯醇复合膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种纳米纤维增强的超顺磁性聚乙烯醇复合膜及其制备方法,其特征在于,向芦苇浆中加氢氧化钠水溶液、硫酸,超声破碎得纳米纤维素晶水溶胶;加热煮沸后,加入FeSO4·7H2O、FeCl3·6H2O,反应后超声分散得负载纳米Fe3O4水溶胶;向碱木质素中加入蒸馏水,得A组分;向壳聚糖中加醋酸配成溶液,加入甘油,与A组分混合;将淀粉、氢氧化钠混合,加去离子水后与聚乙烯醇、硼砂充分混合,反应得交联后的包膜液;将一份成膜液在聚四氟乙烯板上铺膜,风干得底层膜;将负载型水溶胶在底层膜上交替沉积自组装得到磁性负载型夹层;取另一份成膜液在夹层上交替沉积自组装得到另一层膜,制备得到磁膜材料。
Description
技术领域
本发明涉及复合膜领域,具体涉及一种纳米纤维增强的超顺磁性聚乙烯醇复合膜及其制备方法。
背景技术
生物质炭是将农作物秸秆、木屑等生物质材料在限制或隔绝氧气的环境条件下,经热解得到的固体产物。利用农作物秸秆等废弃物制备成的生物质炭由于灰分含量较高,在工业领域应用会受到一定的限制,而在农业领域上却可以广泛应用。
张伟在其硕士学位论文《水稻秸秆炭基缓释肥的制备及性能研究》中,以水稻秸秆为原材料,通过连续热解装置分别在400℃、450℃、500℃、550℃、600℃温度下对水稻秸秆进行热解,制备生物质炭。借助生物质炭的吸附性能,利用圆盘造粒方法制备粒状生物质炭基尿素肥料,生物质炭与尿素质量比1:1、粘结剂添加量为10%、水分的添加量为15-25%,制备的粒状生物质炭基尿素肥料性能较好;利用挤压成型方法制备柱状生物质炭基尿素肥料,粘结剂添加量为7%、生物质炭与尿素质量比1:1、成型压力为6MPa、水分的添加量为5-10%,制备的柱状生物质炭基尿素肥料性能较好。但是存在吸水保水、缓释性能不足。
发明内容
本发明主要解决的技术问题是提供一种纳米纤维增强的超顺磁性聚乙烯醇复合膜及其制备方法,依照该工艺制备的复合膜具备良好的超顺磁性、热稳定性、吸水保水性能及缓释性能。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于,按以下步骤进行:
a. 将10-20重量份芦苇浆机械粉碎后过60-80目筛,1:40-50加入氢氧化钠水溶液,在70-90℃恒温水浴润胀1-2h,过滤、洗涤至中性,与硫酸1:50-60混合,搅拌均匀,在50-60℃水解反应2-3h,离心洗涤至中性,超声破碎1-2h,得纳米纤维素晶水溶胶;
b. 将a中所得水溶胶加热煮沸,加入0.1-0.2g重量份FeSO4·7H2O、0.3-0.5g重量份FeCl3·6H2O,氮气保护下,于60-70℃恒温水浴、机械搅拌,调pH为9-10反应2-3h,升温至80-90℃陈化1-2h后,冷却至室温,离心洗涤至中性,超声分散1-2h,得到负载纳米Fe3O4水溶胶;
c. 向4-8重量份碱木质素中1:10-20加入蒸馏水,60-80℃加热搅拌1-2h,得A组分;向6-10重量份壳聚糖中加入醋酸,配成浓度为3-5%的溶液,加入1-2重量份甘油,与A组分混合,超声振荡1-2h分散均匀;
d. 向6-12重量份淀粉中1:20-30加入去离子水,恒温90-100℃水浴加热搅拌1-2h,使淀粉糊化,加入30-40重量份聚乙烯醇、1-2重量份硼砂及c中所得物料,充分混合、反应1-2h后,得到成膜液,分成两份待用;
e. 将d中所得一份成膜液在平整的聚四氟乙烯板上铺膜,用聚四氟乙烯刮板刮匀,室温下风干,得到底层膜;将b中所得负载型水溶胶,在底层膜上交替沉积自组装得到磁性负载型夹层;取另一份成膜液在负载型夹层上交替沉积自组装得到另一层膜,制备得到磁膜材料。
其中,步骤a中所述氢氧化钠水溶液为5-7mol/L、硫酸质量分数为52-55%;步骤b中所述机械搅拌速度为600-700r/min;步骤e中所述室温下4-6h风干。
本发明的反应机理及有益效果如下:
以芦苇浆为原材料,通过碱预处理、硫酸酸解法和高压均质法,制备得到纳米纤维素晶水溶胶,利用原位合成法将磁性纳米Fe3O4引入水溶胶中,得到负载纳米Fe3O4水溶胶,纳米Fe3O4粒子均匀的分布在复合膜中,制备得到具有良好的超顺磁性、紫外阻隔性、热稳定性和特殊的氧化降解能力的复合膜;木质素具有改良土壤、促进肥效、吸附缓释的效果,壳聚糖抑菌抗菌、自身可降解,可作为肥料缓释载体材料,用甘油对其进行交联改性,能延缓肥料释放时间;用生物可降解性的玉米淀粉、聚乙烯醇为原料,通过添加交联剂(硼砂),与木质素、壳聚糖复合制成膜材料,复合材料在空气中吸水率强,有利于保持水分,提高了缓释效果。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例
一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于,按以下步骤进行:
a. 将20kg芦苇浆机械粉碎后过80目筛,1:40加入氢氧化钠水溶液,在80-90℃恒温水浴润胀1h,过滤、洗涤至中性,与硫酸1:50混合,搅拌均匀,在50-60℃水解反应2h,离心洗涤至中性,超声破碎1h,得纳米纤维素晶水溶胶;
b. 将a中所得水溶胶加热煮沸,加入0.2gkg FeSO4·7H2O、0.5gkg FeCl3·6H2O,氮气保护下,于60-70℃恒温水浴、机械搅拌,调pH为9-10反应2h,升温至80-90℃陈化2h后,冷却至室温,离心洗涤至中性,超声分散1h,得到负载纳米Fe3O4水溶胶;
c. 向8kg碱木质素中1:10加入蒸馏水,70-80℃加热搅拌1h,得A组分;向6kg壳聚糖中加入醋酸,配成浓度为3-5%的溶液,加入1kg甘油,与A组分混合,超声振荡1h分散均匀;
d. 向6kg淀粉中1:20加入去离子水,恒温90-100℃水浴加热搅拌1h,使淀粉糊化,加入40kg聚乙烯醇、1kg硼砂及c中所得物料,充分混合、反应2h后,得到成膜液,分成两份待用;
e. 将d中所得一份成膜液在平整的聚四氟乙烯板上铺膜,用聚四氟乙烯刮板刮匀,室温下风干,得到底层膜;将b中所得负载型水溶胶,在底层膜上交替沉积自组装得到磁性负载型夹层;取另一份成膜液在负载型夹层上交替沉积自组装得到另一层膜,制备得到磁膜材料。
其中,步骤a中所述氢氧化钠水溶液为6mol/L、硫酸质量分数为54%;步骤b中所述机械搅拌速度为650r/min;步骤e中所述室温下5h风干。
Claims (5)
1.一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于:
向芦苇浆中加氢氧化钠水溶液、硫酸,超声破碎得纳米纤维素晶水溶胶;加热煮沸后,加入FeSO4·7H2O、FeCl3·6H2O,反应后超声分散得负载纳米Fe3O4水溶胶;向碱木质素中加入蒸馏水,得A组分;向壳聚糖中加醋酸配成溶液,加入甘油,与A组分混合;将淀粉、氢氧化钠混合,加去离子水后与聚乙烯醇、硼砂充分混合,反应得交联后的包膜液;将一份成膜液在聚四氟乙烯板上铺膜,风干得底层膜;将负载型水溶胶在底层膜上交替沉积自组装得到磁性负载型夹层;取另一份成膜液在夹层上交替沉积自组装得到另一层膜,制备得到磁膜材料。
2.一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于:
将10-20重量份芦苇浆机械粉碎后过60-80目筛,1:40-50加入氢氧化钠水溶液,在70-90℃恒温水浴润胀1-2h,过滤、洗涤至中性,与硫酸1:50-60混合,搅拌均匀,在50-60℃水解反应2-3h,离心洗涤至中性,超声破碎1-2h,得纳米纤维素晶水溶胶;
将a中所得水溶胶加热煮沸,加入0.1-0.2g重量份FeSO4·7H2O、0.3-0.5g重量份FeCl3·6H2O,氮气保护下,于60-70℃恒温水浴、机械搅拌,调pH为9-10反应2-3h,升温至80-90℃陈化1-2h后,冷却至室温,离心洗涤至中性,超声分散1-2h,得到负载纳米Fe3O4水溶胶;
c. 向4-8重量份碱木质素中1:10-20加入蒸馏水,60-80℃加热搅拌1-2h,得A组分;向6-10重量份壳聚糖中加入醋酸,配成浓度为3-5%的溶液,加入1-2重量份甘油,与A组分混合,超声振荡1-2h分散均匀;
d. 向6-12重量份淀粉中1:20-30加入去离子水,恒温90-100℃水浴加热搅拌1-2h,使淀粉糊化,加入30-40重量份聚乙烯醇、1-2重量份硼砂及c中所得物料,充分混合、反应1-2h后,得到成膜液,分成两份待用;
e. 将d中所得一份成膜液在平整的聚四氟乙烯板上铺膜,用聚四氟乙烯刮板刮匀,室温下风干,得到底层膜;将b中所得负载型水溶胶,在底层膜上交替沉积自组装得到磁性负载型夹层;取另一份成膜液在负载型夹层上交替沉积自组装得到另一层膜,制备得到磁膜材料。
3.根据权利要求2所述的一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于,步骤a中所述氢氧化钠水溶液为5-7mol/L、硫酸质量分数为52-55%。
4.根据权利要求2所述的一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于,步骤b中所述机械搅拌速度为600-700r/min。
5.根据权利要求2所述的一种纳米纤维增强的超顺磁性聚乙烯醇复合膜的制备方法,其特征在于,步骤e中所述室温下4-6h风干。
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CN108990972A (zh) * | 2018-05-23 | 2018-12-14 | 北华大学 | 缓释农药薄膜及其制备方法 |
CN110327986A (zh) * | 2019-07-17 | 2019-10-15 | 齐鲁工业大学 | 改性纳米纤维素纤维及制备方法与催化亚甲基蓝降解的应用 |
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