CN105967723A - 一种二氧化硅多孔材料的制备方法 - Google Patents
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Abstract
本发明公开了一种二氧化硅多孔材料的制备方法，以正硅酸乙酯为原料，无水乙醇和去离子水为溶剂，利用多种分散剂使硅离子均匀地存在于大分子络合结构中，且利用合适的分散剂浓度合成出可直接干压成型的干凝胶，经干压后的块体材料经热处理后，即可获得二氧化硅多孔材料；该方法工艺简单、周期短、设备简单、成本低、所得多孔材料的孔隙尺寸及分布可控性高。
Description
技术领域
本发明属于材料技术领域，特别涉及一种二氧化硅多孔材料的制备方法。
背景技术
多孔材料以多孔的形式呈现出表面积大的特点，由于具有多孔、表面积大、活性大、易回收等特点使其广泛应用于高效吸附剂和催化剂中。多孔二氧化硅材料不仅具有比表面积大、表面张力小、气体渗透性高等特点，而且其还具有化学稳定性好、耐高温、绝缘性好、耐候性强、无毒无味等优点，不像多孔炭材料一般出现易燃现象，这使二氧化硅多孔材料具有更好的应用前景。本专利提出一种利用分散剂使硅离子均匀分散于体系中，再利用体系自身所具有的粘度一次成型，使颗粒形成过程与多孔材料结构的形成过程合二为一，一步快速地合成出二氧化硅多孔材料，为二氧化硅多孔材料的制备开拓新的制备方法，用于其推广应用。
发明内容
为了克服上述现有技术的缺点，本发明的目的在于提供一种二氧化硅多孔材料的制备方法，具有生产工艺简单、设备要求简单、周期短的特点。
为了实现上述目的，本发明采用的技术方案是：
一种二氧化硅多孔材料的制备方法，以正硅酸乙酯为原料，无水乙醇和去离子水为溶剂，利用分散剂配制出前驱体溶液，再经凝胶化、干燥、干压和热处理过程获得二氧化硅多孔材料。
所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
所述无水乙醇和去离子水的体积比为(2：1)～(3：1)。
所述分散剂加至溶剂中后，分散剂各组份的浓度范围均为0～0.4mol/L。
所述正硅酸乙酯与柠檬酸的摩尔比为1：(1～1.5)。
所述分散剂加至溶剂中，再加入正硅酸乙酯，溶解后用氨水调节pH值至1～5得前驱体溶液，将前驱体溶液于80～85℃下水浴至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体，再将此干凝胶粉体直接进行干压成型，形成块状坯体材料，最后经热处理即得多孔二氧化硅材料。
所述热处理是在ZnO粉体中进行埋烧，温度为700～1000℃。
与现有技术相比，本发明的有益效果是：与现有技术相比，本发明提供的二氧化硅多孔材料的制备方法中，以乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇等作为分散剂直接进行络合发泡的凝胶化过程，通过控制各物质的浓度，特别是各分散剂的用量，配制出适合直接成型的干凝胶，这不仅可以减少造粒、陈腐的过程，还可使结晶过程与烧结一步完成。结合埋烧的热处理过程，利用有机物的发泡和分解燃烧过程形成二氧化硅多孔材料。这种方法工艺步骤少、制备周期短、设备简单、成本低，且所得二氧化硅多孔材料的孔隙尺寸及分布可控性好。
具体实施方式
下面结合实施例详细说明本发明的实施方式。
实施例1
(1)量取50mL无水乙醇和去离子水并按体积比2：1混合，搅拌均匀，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成，其中聚乙二醇又包括聚乙二醇400、聚乙二醇4000和聚乙二醇6000)加入混合液中，分散剂各组份的浓度控制在0.4mol/L。搅拌溶解后，再加入正硅酸乙酯(其中正硅酸乙酯：柠檬酸(摩尔比)＝1：1)，待其溶解后用氨水(体积浓度25～28％)调节pH值至1～5即获得前驱体溶液。
(2)将前驱体溶液于80℃下水浴至凝胶化，再在160℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(3)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得二氧化硅多孔材料，热处理温度为1000℃。所得二氧化硅多孔材料中二氧化硅颗粒尺寸约为30nm～150nm，间隙尺寸为30nm～100nm。
实施例2
(1)量取50mL无水乙醇和去离子水并按体积比3：1混合，搅拌均匀，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成。)加入混合液中，分散剂各组份的浓度分别控制在0.01、0.1、0.1、0.2、0.3、0.4mol/L，搅拌溶解后，再加入正硅酸乙酯(其中正硅酸乙酯：柠檬酸(摩尔比)＝1：1.5)，待其溶解后用氨水(提交浓度25～28％)调节pH值至1～5即获得前驱体溶液。
(2)将前驱体溶液于85℃下水浴至凝胶化，再在140℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(3)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得二氧化硅多孔材料，热处理温度为700℃。所得二氧化硅多孔材料中二氧化硅颗粒尺寸约为30nm～150nm，间隙尺寸为30nm～100nm。
实施例3
(1)量取50mL无水乙醇和去离子水并按体积比3：1，搅拌均匀，称量一定量的分散剂(由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇、聚乙二醇组成。)加入混合液中，分散剂各组份的浓度分别控制在0.03、0.2、0.2、0.2、0.1、0.4mol/L，搅拌溶解后，再加入正硅酸乙酯(其中正硅酸乙酯：柠檬酸(摩尔比)＝1：1.2)，待其溶解后用氨水(体积浓度25～28％)调节pH值至1～5即获得前驱体溶液。
(2)将前驱体溶液于80℃下水浴至凝胶化，再在150℃下干燥形成干凝胶，室温下自然晾干后将粉体进行研磨过筛。
(3)将过筛后的干粉直接干压成形，形成块状坯体材料，最后将块状坯体材料在ZnO粉体中进行埋烧即获得二氧化硅多孔材料，热处理温度为900℃。所得二氧化硅多孔材料中二氧化硅颗粒尺寸约为30nm～150nm，间隙尺寸为30nm～100nm。
Claims (7)
1.一种二氧化硅多孔材料的制备方法，其特征在于，以正硅酸乙酯为原料，无水乙醇和去离子水为溶剂，利用分散剂配制出前驱体溶液，再经凝胶化、干燥、干压和热处理过程获得二氧化硅多孔材料。
2.根据权利要求1所述二氧化硅多孔材料的制备方法，其特征在于，所述分散剂由乙二胺四乙酸、柠檬酸、二乙烯三胺五羧酸、酒石酸、乙二醇和聚乙二醇组成。
3.根据权利要求1或2所述二氧化硅多孔材料的制备方法，其特征在于，所述无水乙醇和去离子水的体积比为(2：1)～(3：1)。
4.根据权利要求2所述二氧化硅多孔材料的制备方法，其特征在于，所述正硅酸乙酯与柠檬酸的摩尔比为1：(1～1.5)。
5.根据权利要求1或4所述二氧化硅多孔材料的制备方法，其特征在于，所述分散剂加至溶剂中，再加入正硅酸乙酯，溶解后用氨水调节pH值至1～5得前驱体溶液，将前驱体溶液于80～85℃下水浴至凝胶化，再在140～160℃下干燥形成干凝胶，室温下自然晾干后进行研磨过筛得到干凝胶粉体，再将此干凝胶粉体直接进行干压成型，形成块状坯体材料，最后经热处理即得多孔二氧化硅材料。
6.根据权利要求5所述二氧化硅多孔材料的制备方法，其特征在于，所述分散剂加至溶剂中后，分散剂各组份的浓度范围均为0～0.4mol/L。
7.根据权利要求5所述二氧化硅多孔材料的制备方法，其特征在于，所述热处理是在ZnO粉体中进行埋烧，温度为700～1000℃。
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