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CN105967745A - 一种多孔稳态Bi12SiO20块材的制备方法 - Google Patents

一种多孔稳态Bi12SiO20块材的制备方法 Download PDF

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CN105967745A
CN105967745A CN201610292682.7A CN201610292682A CN105967745A CN 105967745 A CN105967745 A CN 105967745A CN 201610292682 A CN201610292682 A CN 201610292682A CN 105967745 A CN105967745 A CN 105967745A
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伍媛婷
栗梦龙
张娟娟
王众
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Shaanxi University of Science and Technology
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Abstract

本发明公开了一种多孔稳态Bi12SiO20块材的制备方法，以氧化铋和正硅酸乙酯为原料，将其与分散剂以一定方式溶于无水乙醇和去离子水混合溶液中，利用分散剂使离子均匀存在于干凝胶粉体中，再将此干凝胶直接压制成型，经热处理即可获得多孔稳态Bi12SiO20块材；该方法制备周期短、工艺设备简单、成本低，由于利用了适当的分散剂配方，所得多孔材料的孔隙尺寸及分布更均匀。

Description

一种多孔稳态Bi12SiO20块材的制备方法
技术领域
本发明属于材料技术领域，特别涉及一种多孔稳态Bi12SiO20块材的制备方法。
背景技术
目前，在Bi2O3-SiO2系统中发现和研究的化合物晶相主要包括三种：Bi12SiO20晶体、Bi4Si3O12晶体和Bi2SiO5晶体,其中Bi12SiO20晶体为一种稳定的晶相，目前制备Bi12SiO20粉体的方法主要有固相法、水热法、溶胶-凝胶法及熔盐法等。多孔块体材料不仅利用细小的孔隙使材料本身保持了较高的比表面积，而且利用块体材料的优势，解决了粉体材料团聚的问题。制备多孔块体材料，传统方法是结合以上方法所得Bi12SiO20粉体，再添加各种物质(如发泡剂、粘结剂等)，经成型和热处理获得多孔块体材料，传统方法周期长、工艺复杂，不利于Bi12SiO20的推广应用。本专利开发了一种一步合成多孔Bi12SiO20块材的方法。
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多孔稳态Bi12SiO20块材的制备方法，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：
一种多孔稳态Bi12SiO20块材的制备方法，包括如下步骤：
(1)将分散剂溶于无水乙醇中，加入正硅酸乙酯搅拌溶解得到溶液A；
(2)将氧化铋溶于硝酸中反应形成溶液B，将溶液B与溶液A混合，调节pH值至2～4获得溶胶B；
(3)将溶胶B于80～85℃下水浴1～3h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；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理得到多孔稳态Bi12SiO20块材。
所述步骤(1)中，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。
所述溶液A中，分散剂各组份的浓度范围均为0～0.8mol/L。
所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(8：1)～(4：1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(1.2～2.0)。
所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为550℃～650℃。
与现有技术相比，本发明的有益效果是：本发明提供的多孔稳态Bi12SiO20块材的制备方法中，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400、聚乙二醇4000、聚乙二醇6000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多孔稳态Bi12SiO20块材。这种方法工艺步骤少、制备周期短、设备简单、成本低，且所得多孔稳态Bi12SiO20块材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
一种多孔稳态Bi12SiO20块材的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，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，分散剂各组份的浓度控制在0.8mol/L)加入其中，搅拌溶解，将正硅酸乙酯加入其中以形成溶液A。
(2)将氧化铋溶于硝酸中反应形成溶液，硝酸以能完全溶解氧化铋为准,将其加入溶液A中，其中，Bi：Si(摩尔比)＝8：1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1.2。用氨水(体积浓度25～28％)调节pH值至2～4即获得溶胶B。
(3)将溶胶B于80℃下水浴1～3h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。
(4)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，即获得多孔稳态Bi12SiO20块材，热处理温度为550℃。所得多孔稳态Bi12SiO20块材中为开孔结构，晶粒尺寸约为150nm～600nm，间隙尺寸为150nm～250nm。
实施例2
一种多孔稳态Bi12SiO20块材的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，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，分散剂各组份的浓度控制在0.8mol/L)加入其中，搅拌溶解，将正硅酸乙酯加入其中以形成溶液A。
(2)将氧化铋溶于硝酸中反应形成溶液，硝酸以能完全溶解氧化铋为准,将其加入溶液A中，其中，Bi：Si(摩尔比)＝4：1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：2。用氨水(体积浓度25～28％)调节pH值至2～4即获得溶胶B。
(3)将溶胶B于85℃下水浴1～3h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。
(4)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，即获得多孔稳态Bi12SiO20块材，热处理温度为650℃。所得多孔稳态Bi12SiO20块材中为开孔结构，晶粒尺寸约为150nm～600nm，间隙尺寸为150nm～250nm。
实施例3
一种多孔稳态Bi12SiO20块材的制备方法，包括如下步骤：
(1)量取50mL无水乙醇，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，分散剂各组份的浓度控制在0.01、0.1、0.1、0.5、0.7、0.8mol/L)加入其中，搅拌溶解，将正硅酸乙酯加入其中以形成溶液A。
(2)将氧化铋溶于硝酸中反应形成溶液，硝酸以能完全溶解氧化铋为准,将其加入溶液A中，其中，Bi：Si(摩尔比)＝6：1，Si离子与Bi离子之和：柠檬酸(摩尔比)＝1：1.5。用氨水(体积浓度25～28％)调节pH值至2～4即获得溶胶B。
(3)将溶胶B于80℃下水浴1～3h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。
(4)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，即获得多孔稳态Bi12SiO20块材，热处理温度为600℃。所得多孔稳态Bi12SiO20块材中为开孔结构，晶粒尺寸约为150nm～600nm，间隙尺寸为150nm～250nm。

Claims (5)

1.一种多孔稳态Bi12SiO20块材的制备方法，其特征在于，包括如下步骤：
(1)将分散剂溶于无水乙醇中，加入正硅酸乙酯搅拌溶解得到溶液A；
(2)将氧化铋溶于硝酸中反应形成溶液B，将溶液B与溶液A混合，调节pH值至2～4获得溶胶B；
(3)将溶胶B于80～85℃下水浴1～3h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；
(4)将过筛后的干粉直接干压成型，形成块状坯体材料，最后将块状坯体材料进行热处理，得到多孔稳态Bi12SiO20块材。
2.根据权利要求1所述多孔稳态Bi12SiO20块材的制备方法，其特征在于，所述步骤(1)中，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2所述多孔稳态Bi12SiO20块材的制备方法，其特征在于，所述溶液A中，分散剂各组份的浓度范围均为0～0.8mol/L。
4.根据权利要求2所述多孔稳态Bi12SiO20块材的制备方法，其特征在于，所述正硅酸乙酯和氧化铋的用量满足Bi与Si的摩尔比为(8：1)～(4：1)，且Si离子与Bi离子之和与柠檬酸的摩尔比为1：(1.2～2.0)。
5.根据权利要求1所述多孔稳态Bi12SiO20块材的制备方法，其特征在于，所述步骤(4)中，所述热处理是在ZnO粉体中进行埋烧，温度为550℃～650℃。
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CN107199030A (zh) * 2017-06-30 2017-09-26 常州豫春化工有限公司 一种蜂窝状多孔氧化铋的制备方法

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