CN109967042B - 一种利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料 - Google Patents
一种利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料 Download PDFInfo
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Abstract
本发明公开了一种利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料。本发明中以碱溶壳聚糖溶液作为连续相，有机溶剂作为分散相，非离子表面活性剂作为乳液助稳定剂，混合搅拌，通过超声使内部乳液均匀分散，加热使碱溶壳聚糖溶液原位凝胶化，最后通过透析、冻干后即得壳聚糖气凝胶材料。本发明制备的气凝胶吸附材料，不仅具有大量相互连通的孔道结构，而且还具有良好的压缩回弹性和生物降解性，有望应用于水处理领域，实现对金属离子、染料等的吸附，并且材料具有可重复使用性能，在完全使用后可实现降解。
Description
技术领域
本发明属于气凝胶材料制备领域，涉及一种壳聚糖气凝胶制备方法，具体涉及一种利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料。
背景技术
随着工业废水排放的增加，对于具有高吸附能力的材料的需求越来越大。但是现有吸附材料，如活性炭、硅藻土、吸附树脂等，虽然吸附效果较好，但是存在成本高、回收利用能力低下、制备工艺繁琐、难以降解等缺点。
气凝胶是一类具有三维多孔结构的新型固态材料，具有超低密度、高孔隙率和高比表面积等特点，因而被广泛地应用于吸附、储能、隔音降噪、隔热和催化等领域。
壳聚糖是甲壳素脱乙酰化后的产物，是自然界中储量仅次于纤维素的第二大天然高分子材料，是唯一一种可生物再生的碱性多糖类生物高分子，具有生物相容性好、可生物降解、无毒等特点，可被广泛地应用于生物医疗产业、农业、食品工业、纺织工业、环境保护等领域。
如果将壳聚糖作为原料用于制备气凝胶，可以结合壳聚糖本身具有的特点和气凝胶材料的结构特点，有望得到一种具有高吸附性能、可降解，且环境友好的吸附材料。
发明内容
本发明的目的是利用乳液模板法的特点，制备一种具有多孔结构的壳聚糖吸附材料，以提高其吸附能力和重复使用能力，并且在完全使用后可实现生物降解。
本发明提供以下技术方案实现：
以碱溶壳聚糖溶液作为连续相，有机溶剂作为分散相，非离子表面活性剂作为乳液助稳定剂，实现以乳液模板法制备壳聚糖气凝胶吸附材料。其具体制备工艺为：
首先使用一水合氢氧化锂和尿素作为溶剂，利用冷冻爆破法溶解壳聚糖得到一定量碱溶壳聚糖溶液，再向上述溶液中加入有机分散相和乳液助稳定剂，搅拌混合获得混合溶液，通过超声使内部乳液均匀分散，最后将上述乳液混合物转移至60℃烘箱内加热2小时，使其中的连续相(碱溶壳聚糖溶液)原位凝胶，经透析去除分散相乳液，冻干后得到壳聚糖气凝胶吸附材料。上述技术方案中，所述的混合溶液中碱溶壳聚糖溶液的用量为75-93wt％、分散相的用量为5-20wt％、乳液助稳定剂的用量为2-20wt％。
所述碱溶壳聚糖溶液的制备工艺(冷冻-爆破法)为：按照质量百分比，将壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水，混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；所述的壳聚糖分子量为200000-2500000。
所述分散相为液体石蜡油、正己烷、环己烷、正庚烷、正辛烷中的至少一种。
所述乳液助稳定剂为山梨糖醇脂肪酸酯、失水山梨糖醇脂肪酸酯(span-80)、聚氧乙烯脱水山梨醇单油酸酯(吐温80)、聚环氧乙烯烷基胺、甘油脂肪酸中的至少一种。
所述搅拌速度为400-2000r/min，搅拌时间为30-150min。
所述超声功率为100W，超声时间为30-150min。
相对于现有技术，本发明具有以下优点：
1.本发明使用壳聚糖作为原料，存在大量的氨基、羟基等活性基团，同时采用乳液模板法制备气凝胶材料，赋予材料大量的通孔结构，可以实现对金属离子、染料等有效快速的吸附；
2.本发明中采用碱溶壳聚糖溶液作为连续相，巧妙地将碱溶壳聚糖溶液加热发生凝胶化的特点与乳液模板法相结合：碱溶壳聚糖呈溶液状态时，分散相乳液可以通过搅拌和超声实现分散；当碱溶壳聚糖凝胶时，分散相乳液被凝胶所固定；最后通过透析去除分散相乳液，乳液占据的空间在冻干后成为孔结构。无需使用交联剂，安全环保；
3.本发明采用壳聚糖作为原料，具有生物降解性能，在完全使用后可实现降解，对环境无污染。
附图说明
图1是本发明制得的碱溶壳聚糖基气凝胶吸附材料示意图；
图2是本发明制得的碱溶壳聚糖基气凝胶吸附材料SEM图。
具体实施方式
结合以下实例进一步说明本发明。
实施例1：
1.按照如下质量百分比称取各组分：壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水；所述的壳聚糖分子量为1500000；将上述组分混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；
2.取80g步骤1)中制得的碱溶壳聚糖溶液，加入15g液体石蜡，5g失水山梨糖醇脂肪酸酯，在400r/min转速下搅拌30min，混合物转移至超声仪中超声60min，再置于60℃烘箱内加热2小时使壳聚糖溶液原位凝胶化，然后依次使用石油醚、水进行透析除去分散相乳液，最后冻干得到壳聚糖气凝胶吸附材料。
3.该气凝胶经氮气吸附-解吸附测试测得比表面积为143.58m2/g。
实施例2：
1.按照如下质量百分比称取各组分：壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水；所述的壳聚糖分子量为2200000；将上述组分混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；
2.取75g步骤1)中制得的碱溶壳聚糖溶液，加入20g正己烷，5g山梨糖醇脂肪酸酯，在1000r/min转速下搅拌60min，混合物转移至超声仪中超声80min，再置于60℃烘箱内加热2小时使壳聚糖溶液完全凝胶化，然后依次使用石油醚、水进行透析除去分散相乳液，最后冻干得到壳聚糖气凝胶吸附材料。
3.该气凝胶经氮气吸附-解吸附测试测得比表面积为157.37m2/g。
实施例3：
1.按照如下质量百分比称取各组分：壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水；所述的壳聚糖分子量为1800000；将上述组分混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；
2.取82g步骤1)中制得的碱溶壳聚糖溶液，加入15g环己烷，3g聚环氧乙烯烷基胺，在600r/min转速下搅拌100min，混合物转移至超声仪中超声60min，再置于60℃烘箱内加热2小时使壳聚糖溶液完全凝胶化，然后依次使用石油醚、水进行透析除去分散相乳液，最后冻干得到壳聚糖气凝胶吸附材料。
3.该气凝胶经氮气吸附-解吸附测试测得比表面积为178.57m2/g。
实施例4：
1.按照如下质量百分比称取各组分：壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水；所述的壳聚糖分子量为1000000；将上述组分混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；
2.取86g步骤1)中制得的碱溶壳聚糖溶液，加入8g正庚烷，6g甘油脂肪酸，在1500r/min转速下搅拌30min，混合物转移至超声仪中超声120min，再置于60℃烘箱内加热2小时使壳聚糖溶液完全凝胶化，然后依次使用石油醚、水进行透析除去分散相乳液，最后冻干得到壳聚糖气凝胶吸附材料。
3.该气凝胶经氮气吸附-解吸附测试测得比表面积为159.25m2/g。
实施例5：
1.按照如下质量百分比称取各组分：壳聚糖4％、一水合氢氧化锂8％、尿素6％，其余为水；所述的壳聚糖分子量为800000；将上述组分混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；
2.取90g步骤1)中制得的碱溶壳聚糖溶液，加入7g正辛烷，3g聚氧乙烯脱水山梨醇单油酸酯，在500r/min转速下搅拌150min，混合物转移至超声仪中超声120min，再置于60℃烘箱内加热2小时使壳聚糖溶液完全凝胶化，然后依次使用石油醚、水进行透析除去分散相乳液，最后冻干得到壳聚糖气凝胶吸附材料。
3.该气凝胶经氮气吸附-解吸附测试测得比表面积为120.33m2/g。
Claims (5)
1.利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料，其特征在于，该材料的制备是：以碱溶壳聚糖溶液作为连续相，有机溶剂作为分散相，非离子表面活性剂作为乳液助稳定剂，搅拌混合获得混合溶液，通过超声使内部乳液均匀分散，加热使碱溶壳聚糖溶液原位凝胶化，经透析去除分散相乳液，最后冻干即得碱溶壳聚糖基气凝胶吸附材料；所述的混合溶液中碱溶壳聚糖溶液的用量为75-93wt%、分散相的用量为5-20wt%、乳液助稳定剂的用量为2-20wt%；所述的搅拌速度为400-2000r/min，搅拌时间为30-150min；所述的超声功率为100W，超声时间为30-150min。
2.如权利要求1所述的利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料，其特征在于：首先使用一水合氢氧化锂和尿素作为溶剂，利用冷冻爆破法溶解壳聚糖得到碱溶壳聚糖溶液，再向上述溶液中加入有机分散相和乳液助稳定剂，搅拌混合获得混合溶液，通过超声使内部乳液均匀分散，最后将上述乳液混合物转移至60℃烘箱内加热2小时，使其中的连续相碱溶壳聚糖溶液原位凝胶，经透析去除分散相乳液，冻干后得到碱溶壳聚糖基气凝胶吸附材料。
3.如权利要求1或2所述利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料，其特征在于：所述的碱溶壳聚糖溶液的制备工艺具体为：按照质量百分比，将壳聚糖4%、一水合氢氧化锂8%、尿素6%，其余为水，混合溶胀后，经多次冷冻-解冻过程制备得到碱溶壳聚糖溶液；所述的壳聚糖分子量为200000-2500000。
4.如权利要求1或2所述利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料，其特征在于：所述的分散相为液体石蜡油、正己烷、环己烷、正庚烷、正辛烷中的至少一种。
5.如权利要求1或2所述利用乳液模板法制备的碱溶壳聚糖基气凝胶吸附材料，其特征在于：所述的乳液助稳定剂为山梨糖醇脂肪酸酯、失水山梨糖醇脂肪酸酯（span-80）、聚氧乙烯脱水山梨醇单油酸酯（吐温80）中的至少一种。
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Inventor after: Jin Xiaoqiang Inventor after: Jiang Huihong Inventor after: Bao Xiaojiong Inventor after: Fu Beijia Inventor after: Jiang Zhiqi Inventor after: Hu Qiaoling Inventor after: Wang Zhengke Inventor before: Wang Zhengke Inventor before: Jin Xiaoqiang Inventor before: Jiang Huihong Inventor before: Bao Xiaojiong Inventor before: Fu Beijia Inventor before: Jiang Zhiqi Inventor before: Hu Qiaoling |