CN107694490B - 一种硅-铁复合气凝胶的制备方法 - Google Patents
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Abstract
本发明公开了一种气凝胶的制备方法，具体是指一种硅‑铁复合气凝胶的制备方法，包括二氧化硅‑氧化铁气凝胶和二氧化硅‑铁气凝胶;其特征在于：以酸性硅溶胶为原料，以氢氧化钠或碳酸钠、碳酸氢钠、氨的水溶液为凝胶催化剂，以铁盐作为铁源和凝胶促进剂，在水相中凝胶，然后用乙醇进行溶剂置换，同时老化；以六甲基二硅氮烷的六甲基二硅氧烷溶液作为改性剂，改性完成后得SiO2‑Fe2O3气凝胶块体。进一步用氢气还原，即可制得SiO2‑Fe气凝胶。本发明以价格低廉的无机硅源——酸性硅溶胶为原料，生产成本更低，而制备的气凝胶性能更佳。
Description
技术领域：
本发明涉及一种气凝胶的制备方法，具体是指一种硅-铁复合气凝胶的制备方法，包括二氧化硅-氧化铁(SiO2-Fe2O3)气凝胶和二氧化硅-铁(SiO2-Fe)气凝胶。
背景技术：
二氧化硅(SiO2)气凝胶因其独特的三维网络结构、气体分散介质以及纳米量级的固体相和孔隙结构使其具有低密度、高比表面积、高孔隙率等特点，引起人们极大的兴趣，可用来作为保温隔热、隔音、吸附、催化剂载体、声阻耦合等材料，应用开发已比较成熟。为了进一步拓展硅气凝胶的应用，复合气凝胶的研发正方兴未艾，硅-铝(SiO2-Al2O3)复合气凝胶、硅-锆(SiO2-ZrO2)复合气凝胶、硅-钛(SiO2-TiO2)复合气凝胶、硅-碳(SiO2-C)复合气凝胶以及硅与有机物复合气凝胶等被相继制备，硅-铁复合气凝胶是一种含纳米级的金属铁、氧化铁的、具有铁磁性的复合气凝胶，其独特的三维网络多孔结构能够保证磁性纳米颗粒的均匀分散，限制颗粒的团聚和长大，同时通过控制颗粒在凝胶内部的分散，能够有效地调节材料的磁性，可应用于生产磁光传感器、生物感应元件等磁性器件，在催化领域也有潜在的应用前景，含单质铁的硅-铁复合气凝胶是优质的还原剂，对硝基苯、氯代芳香族化合物、六价铬、二价铅、三价砷等具有优越的还原性和还原效率，是很有前景的污染物处理和土壤修复剂。
硅-铁复合气凝胶的制备方法，目前主要有以下几种：
1、以乙醇为溶剂，铁或铁的氧化物纳米颗粒与正硅酸乙酯(或正硅酸甲酯、甲基三乙氧基硅烷)水解的二氧化硅溶胶混合，经过凝胶、老化、和超临界干燥，得到复合气凝胶。由于铁或铁的氧化物纳米颗粒大小、均匀性以及在溶胶中的分散性难以控制，得到的复合气凝胶性能不稳定，重现性差。
2、用铁盐(硝酸铁、铁的EDTA络合物、醋酸亚铁等)水溶液与正硅酸乙酯(或正硅酸甲酯、甲基三乙氧基硅烷)的乙醇溶液共水解，加碱凝胶、老化、超临界干燥得到复合气凝胶。
3、用铁盐(硝酸铁、铁的EDTA络合物、醋酸亚铁等)与正硅酸乙酯(或正硅酸甲酯、甲基三乙氧基硅烷)的乙醇溶液共水解，加碱凝胶、老化，最后用六甲基二硅氮烷的正己烷溶液改性，常压干燥得到复合气凝胶。但常压干燥过程时间长、效率低，干燥残液成分复杂，回收困难。
发明内容：
本发明的目的在于提供一种工艺简单、效率高、性能优良、溶剂易于回收且可重复使用的常压干燥硅-铁复合气凝胶的方法。
本发明采取的技术方案如下：
一种硅-铁复合气凝胶的制备方法，其特征在于：以酸性硅溶胶为原料，以氢氧化钠或碳酸钠、碳酸氢钠、氨的水溶液为凝胶催化剂，以铁盐本身作为凝胶促进剂，在水相中凝胶，然后用乙醇进行溶剂置换，同时老化；以六甲基二硅氮烷的六甲基二硅氧烷溶液作为改性剂，改性完成后得SiO2-Fe2O3气凝胶块体。
作为进一步优选的设置：
采用质量含量20％二氧化硅的酸性硅溶胶为硅源，采用质量含量6-15％的硝酸铁水溶液为凝胶促进剂，酸性硅溶胶与硝酸铁水溶液的质量比为1：1～1.5.
改性剂的用量为：1/5～15g/ml(酸性硅溶胶/改性剂)。
所述的凝胶，采用质量含量5％的氨水，调节PH值为7.2，在70℃下静置2小时后凝胶。
所述的置换，在70℃下采用体积含量95％的乙醇置换两次。
改性完成后，常压干燥并回收六甲基二硅氧烷，得到六甲基二硅氮烷的六甲基二硅氧烷溶液，回收重复使用。
改性完成后，得到的SiO2-Fe2O3气凝胶块体，置于管式炉中，通入氢气，同时逐渐升温至500℃，维持2小时，得褐色SiO2-Fe复合气凝胶。
更进一步的：
一种硅-铁复合气凝胶的制备方法，其特征在于：量取100克含质量含量20％二氧化硅的酸性硅溶胶(PH值为2.2)，加入100毫升质量含量8％的硝酸铁水溶液，快速搅拌下滴加质量含量5％的氨水至PH值为7.2,70℃下静置2小时后凝胶，先用1000毫升70℃的水浸泡1小时，再用70℃的体积含量95％的乙醇置换两次，每次用量1000毫升，接着用1000毫升质量分数为20％的六甲基二硅氮烷的六甲基二硅氧烷溶液改性2小时，常压干燥并回收六甲基二硅氧烷，得SiO2-Fe2O3的棕色半透明气凝胶块体。
取上述SiO2-Fe2O3气凝胶块体于管式炉中，通入氢气，同时逐渐升温至500℃，维持2小时，得褐色SiO2-Fe复合气凝胶。
本发明的有益效果如下：
1、以价格低廉的无机硅源——酸性硅溶胶为原料，生产成本更低，而制备的气凝胶性能更佳；
2、以氢氧化钠(或碳酸钠、碳酸氢钠、氨水)水溶液为凝胶催化剂，以铁盐本身作为凝胶促进剂，减少了助剂的使用；
3、在水相中凝胶，凝胶结构更为均匀；
4、以体积含量95％乙醇进行溶剂置换，同时老化，工艺过程更为简单；
5、以六甲基二硅氮烷的六甲基二硅氧烷溶液(HMDZ/MM)作为改性剂，六甲基二硅氮烷改性后生成六甲基二硅氧烷，无需分离，直接回收和重复使用，对环境友好。
具体实施方式：
以下结合具体实施方式，对本发明作进一步说明。
实施例1：
量取100克含20％(质量含量)二氧化硅的酸性硅溶胶(PH值为2.2)，加入100克8％(质量含量)的硝酸铁水溶液，快速搅拌下滴加5％(质量含量)的氨水至PH值为7.2,70℃下静置2小时后凝胶，先用1000毫升70℃的水浸泡1小时，再用70℃的95％(体积含量)的乙醇置换两次，每次用量1000毫升，接着用1000毫升质量分数为20％的六甲基二硅氮烷的六甲基二硅氧烷溶液改性2小时，常压干燥并回收六甲基二硅氧烷，得SiO2-Fe2O3的棕色半透明气凝胶块体。
取上述SiO2-Fe2O3气凝胶块体于管式炉中，通入氢气，同时逐渐升温至500℃，维持2小时，得褐色SiO2-Fe复合气凝胶。
对比实施例1：制备方法与上述相同，区别在于：采用69.4克正硅酸乙酯为硅源，加30.6克水，再加1毫升65％的硝酸水解获得凝胶前体(二氧化硅含量相同)，制备SiO2-Fe2O3气凝胶。
性能对照：
将实施例1和对比实施例1进行性能对照如表1所示：
表1、
分析：如表1所示，本发明采用价格低廉的无机硅源——酸性硅溶胶为原料，替代现有常用的正硅酸乙酯硅源，不仅从成本上大大降低，而且从制备的气凝胶性能分析，与现有制备的气凝胶性能相当或在某些方面有所提升。
实施例2-4：
制备方法同实施例1，区别在于：调整凝胶催化剂、硝酸铁的用量，并检测其对气凝胶性能的影响。
表2：
分析：如表2所示：
1、本发明以氢氧化钠(或碳酸钠、碳酸氢钠、氨水)水溶液为凝胶催化剂，以铁盐本身作为凝胶促进剂；这样可以减少凝胶促进剂的使用，同时，从制备的气凝胶性能分析，与现有制备的气凝胶性能相比，在某些方面有所提升。
2、通过控制凝胶催化剂和硝酸铁含量，可以获得更佳的复合气凝胶性能，如表2所示：硝酸铁含量较低，则制备的气凝胶的铁含量低、铁磁性较弱，直接影响复合气凝胶的性能与应用，而硝酸铁含量过高，会导致铁或氧化铁的团聚，形成较大的铁或氧化铁颗粒，从而影响复合气凝胶性能，我们通过反复实验证实：硝酸铁含量控制在6-15％时，可以获得较好的复合气凝胶性能，尤其是硝酸铁含量为8％时，效果为最佳。
实施例5：
制备方法同实施例1，区别在于：采用实施例1回收的六甲基二硅氧烷，回收后直接作为改性剂的溶剂继续用于气凝胶的制备。
表3：
分析：如表3所示，本发明采用以六甲基二硅氮烷的六甲基二硅氧烷溶液(HMDZ/MM)作为改性剂，六甲基二硅氮烷改性后生成六甲基二硅氧烷，无需分离，直接回收和重复使用，经实验证实，上述溶剂回收利用5-10次后仍有很好的改性效果，从而大大节约了成本，减少了有机废弃物的排放，具有非常好的环保效果。
Claims (1)
1.一种硅-铁复合气凝胶的制备方法，其特征在于：量取100克含质量含量20%二氧化硅的酸性硅溶胶pH值为2.2，加入100毫升质量含量8%的硝酸铁水溶液，快速搅拌下滴加质量含量5%的氨水至PH值为7.2,70℃下静置2小时后凝胶，先用1000毫升70℃的水浸泡1小时，再用70℃的体积含量95%的乙醇置换两次，每次用量1000毫升，接着用1000毫升质量分数为20%的六甲基二硅氮烷的六甲基二硅氧烷溶液改性2小时，常压干燥并回收六甲基二硅氧烷，得SiO2- Fe2O3的棕色半透明气凝胶块体；
取上述SiO2- Fe2O3气凝胶块体于管式炉中，通入氢气，同时逐渐升温至500℃，维持2小时，得褐色SiO2- Fe复合气凝胶。
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