CN105967723A - Preparation method of silica porous material - Google Patents
Preparation method of silica porous material Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000011148 porous material Substances 0.000 title abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000011975 tartaric acid Substances 0.000 claims description 6
- 235000002906 tartaric acid Nutrition 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001879 gelation Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 125000003827 glycol group Chemical group 0.000 claims 1
- 239000002210 silicon-based material Substances 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- -1 silicon ions Chemical class 0.000 abstract description 2
- 239000013590 bulk material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 229940057838 polyethylene glycol 4000 Drugs 0.000 description 1
- 229940093429 polyethylene glycol 6000 Drugs 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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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。The invention discloses a method for preparing a silicon dioxide porous material, which uses ethyl orthosilicate as a raw material, absolute ethanol and deionized water as a solvent, and uses various dispersants to make silicon ions evenly exist in macromolecular complexes Structure, and use the appropriate dispersant concentration to synthesize xerogels that can be directly dry-pressed, and the dry-pressed bulk material can be heat-treated to obtain silica porous materials; this method is simple in process and short in cycle , simple equipment, low cost, high controllability of pore size and distribution of the obtained porous material.
Description
技术领域technical field
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。The invention belongs to the technical field of materials, and in particular relates to a preparation method of a silicon dioxide porous material.
背景技术Background technique
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。Porous materials have the characteristics of large surface area in the form of pores, and are widely used in high-efficiency adsorbents and catalysts due to their porous, large surface area, high activity, and easy recovery. Porous silica materials not only have the characteristics of large specific surface area, small surface tension, and high gas permeability, but also have the advantages of good chemical stability, high temperature resistance, good insulation, strong weather resistance, non-toxic and tasteless, unlike porous silica materials. Carbon materials are generally flammable, which makes silica porous materials have better application prospects. This patent proposes a method of using a dispersant to uniformly disperse silicon ions in the system, and then using the viscosity of the system itself to shape it at one time, so that the particle formation process and the formation process of the porous material structure are combined into one, and the two can be quickly synthesized in one step. The silicon oxide porous material develops a new preparation method for the preparation of the silicon dioxide porous material and is used for its popularization and application.
发明内容Contents of the invention
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。In order to overcome the above-mentioned shortcomings of the prior art, the object of the present invention is to provide a method for preparing a silica porous material, which has the characteristics of simple production process, simple equipment requirements and short cycle time.
为了实现上述目的，本发明采用的技术方案是：In order to achieve the above object, the technical scheme adopted in the present invention is:
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。A method for preparing a silicon dioxide porous material, using ethyl orthosilicate as a raw material, absolute ethanol and deionized water as a solvent, using a dispersant to prepare a precursor solution, and then gelling, drying, dry pressing and The heat treatment process obtains a silica porous material.
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。The dispersant is composed of ethylenediaminetetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, tartaric acid, ethylene glycol and polyethylene glycol.
所述无水乙醇和去离子水的体积比为(2：1)～(3：1)。The volume ratio of the absolute ethanol to deionized water is (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。After the dispersant is added into the solvent, the concentration range of each component of the dispersant is 0-0.4mol/L.
所述正硅酸乙酯与柠檬酸的摩尔比为1：(1～1.5)。The molar ratio of tetraethyl orthosilicate to citric acid is 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。Add the dispersant to the solvent, then add tetraethyl orthosilicate, adjust the pH value to 1-5 with ammonia water after dissolving to obtain a precursor solution, put the precursor solution in a water bath at 80-85°C until gelation, and then Dried at 140-160°C to form a xerogel, dried naturally at room temperature, ground and sieved to obtain a xerogel powder, and then directly dry-pressed the xerogel powder to form a block-shaped green body material, Finally, the porous silica material is obtained by heat treatment.
所述热处理是在ZnO粉体中进行埋烧，温度为700～1000℃。The heat treatment is to bury and burn ZnO powder at a temperature of 700-1000°C.
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。Compared with the prior art, the beneficial effects of the present invention are: compared with the prior art, in the preparation method of the silica porous material provided by the present invention, ethylenediaminetetraacetic acid, citric acid, diethylenetriaminepenta Carboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol, etc. are used as dispersants to directly carry out the gelation process of complexation and foaming. By controlling the concentration of each substance, especially the amount of each dispersant, a compound suitable for direct molding can be prepared. Xerogel, which can not only reduce the process of granulation and decay, but also complete the crystallization process and sintering in one step. Combined with the heat treatment process of burying, the porous material of silica is formed by the foaming and decomposition combustion process of organic matter. The method has few process steps, short preparation period, simple equipment and low cost, and the pore size and distribution of the obtained silicon dioxide porous material are well controllable.
具体实施方式detailed description
下面结合实施例详细说明本发明的实施方式。The implementation of the present invention will be described in detail below in conjunction with the examples.
实施例1Example 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。(1) Measure 50mL of absolute ethanol and deionized water and mix them at a volume ratio of 2:1, stir evenly, weigh a certain amount of dispersant (made of ethylenediaminetetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid , tartaric acid, ethylene glycol, polyethylene glycol, wherein polyethylene glycol includes polyethylene glycol 400, polyethylene glycol 4000 and polyethylene glycol 6000) added to the mixed solution, the concentration of each component of the dispersant Controlled at 0.4mol/L. After stirring and dissolving, add ethyl orthosilicate (wherein ethyl orthosilicate: citric acid (molar ratio) = 1:1), after it dissolves, adjust the pH value to 1 with ammonia water (volume concentration 25-28%) ~5 to obtain the precursor solution.
(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。(2) Put the precursor solution in a water bath at 80°C until it gels, and then dry it at 160°C to form a xerogel. After drying naturally at room temperature, the powder is ground and sieved.
(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。(3) The sieved dry powder is directly dry-pressed to form a block-shaped green body material, and finally the block-shaped green body material is buried and fired in ZnO powder to obtain a silica porous material, and the heat treatment temperature is 1000°C. The silicon dioxide particle size in the obtained silicon dioxide porous material is about 30nm-150nm, and the gap size is 30nm-100nm.
实施例2Example 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。(1) Measure 50mL of absolute ethanol and deionized water and mix them at a volume ratio of 3:1, stir evenly, weigh a certain amount of dispersant (made of ethylenediaminetetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid , tartaric acid, ethylene glycol, polyethylene glycol.) into the mixed solution, the concentration of each component of the dispersant is controlled at 0.01, 0.1, 0.1, 0.2, 0.3, 0.4mol/L, after stirring to dissolve, then add Ethyl orthosilicate (wherein ethyl orthosilicate: citric acid (molar ratio) = 1:1.5), after it is dissolved, adjust the pH value to 1-5 with ammonia water (concentration submitted: 25-28%) to obtain the precursor solution.
(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。(2) Put the precursor solution in a water bath at 85°C until gelation, and then dry at 140°C to form a xerogel. After drying naturally at room temperature, the powder is ground and sieved.
(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。(3) The sieved dry powder is directly dry-pressed to form a block-shaped green body material, and finally the block-shaped green body material is buried and fired in ZnO powder to obtain a silica porous material, and the heat treatment temperature is 700°C. The silicon dioxide particle size in the obtained silicon dioxide porous material is about 30nm-150nm, and the gap size is 30nm-100nm.
实施例3Example 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。(1) Measure 50mL of absolute ethanol and deionized water at a volume ratio of 3:1, stir evenly, and weigh a certain amount of dispersant (made of ethylenediaminetetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, Tartaric acid, ethylene glycol, polyethylene glycol.) into the mixed solution, the concentration of each component of the dispersant is controlled at 0.03, 0.2, 0.2, 0.2, 0.1, 0.4mol/L, after stirring and dissolving, add normal Ethyl silicate (wherein tetraethyl orthosilicate: citric acid (molar ratio) = 1:1.2), after it is dissolved, use ammonia water (volume concentration 25-28%) to adjust the pH value to 1-5 to obtain the precursor solution .
(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。(2) Put the precursor solution in a water bath at 80°C until it gels, and then dry it at 150°C to form a xerogel. After drying naturally at room temperature, the powder is ground and sieved.
(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。(3) The sieved dry powder is directly dry-pressed to form a block-shaped green body material, and finally the block-shaped green body material is buried and fired in ZnO powder to obtain a silica porous material, and the heat treatment temperature is 900°C. The silicon dioxide particle size in the obtained silicon dioxide porous material is about 30nm-150nm, and the gap size is 30nm-100nm.
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