CN100400153C - Preparation method of composite adsorption filter material containing porous airgel - Google Patents
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 16
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 11
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- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
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- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及复合吸附过滤材料及其制备方法领域，特别涉及含多孔气凝胶的复合吸附过滤材料及其制备方法领域。The invention relates to the field of composite adsorption filter material and its preparation method, in particular to the field of composite adsorption filter material containing porous airgel and its preparation method.
背景技术Background technique
SiO2气凝胶是一种高比表面积、低密度的多孔材料。由于纳米网络结构的存在，导致了这种材料本身具有特殊的性质，在光学、电学、声学、环保、冶金等众多领域有着广泛的应用前景，被美国第250期《科学》列为世界十大热门科学技术。我国也有许多人在进行这方面的研究。SiO2纳米多孔气凝胶具有很高的比表面和空洞率，是一种轻质高效吸附过滤材料，但实际使用不多，这主要是由于气凝胶的机械强度不够，成型困难，因此阻碍了大面积或大范围广泛使用。为解决这个问题有人尝试用气凝胶与其它材料复合(中国专利95197068.2《一种含有气凝胶的复合材料、其制备方法和应用》，96196879.6《含有气凝胶和粘合剂的复合材料，其制备方法及其应用》，96196880.X《含有纤维的气凝胶复合材料》)，但其制品多为复合板材，许多复合材料会包覆气凝胶的气孔，故基本都用于保温隔热领域，而不用于吸附隔热领域。中国专利8805195.8《气凝胶作为吸附剂的应用》中的气凝胶用作从液相吸附中的吸附剂，但只是在液相吸附应用方面，没有谈到气凝胶的制备和与其他材料复合的问题，以及对复杂气体的吸附过滤作用。SiO 2 airgel is a kind of porous material with high specific surface area and low density. Due to the existence of the nano-network structure, this material itself has special properties, and has broad application prospects in many fields such as optics, electricity, acoustics, environmental protection, metallurgy, etc. Hot science and technology. There are also many people in our country who are doing research in this area. SiO 2 nanoporous airgel has a high specific surface area and void ratio, and is a lightweight and highly efficient adsorption filter material, but it is not used much in practice, mainly because the mechanical strength of the airgel is not enough and the molding is difficult, so it hinders Widely used in a large area or a large range. In order to solve this problem, someone tries to compound airgel with other materials (Chinese patent 95197068.2 "a composite material containing airgel, its preparation method and application", 96196879.6 "composite material containing airgel and adhesive, Its Preparation Method and Its Application", 96196880.X "Aerogel Composite Materials Containing Fibers"), but its products are mostly composite plates, and many composite materials will cover the pores of airgel, so they are basically used for thermal insulation Thermal field, not for adsorption and heat insulation field. The airgel in Chinese patent 8805195.8 "Airgel as Adsorbent Application" is used as an adsorbent from liquid phase adsorption, but only in the application of liquid phase adsorption, there is no mention of the preparation of airgel and the combination with other materials Composite problems, and the adsorption and filtration of complex gases.
发明内容Contents of the invention
本发明的目的在于提供一种应用范围广泛的含多孔气凝胶的复合吸附过滤材料。The purpose of the present invention is to provide a composite adsorption filter material containing porous airgel with a wide range of applications.
本发明的另一个目的在于提供上述复合吸附过滤材料的制备方法。Another object of the present invention is to provide a preparation method of the above-mentioned composite adsorption filter material.
本发明所述的含多孔气凝胶的复合吸附过滤材料，其中所含的气凝胶与有机或无机的纤维或织物都具有吸附性能，两者含量可根据实际应用需要进行调节。气凝胶含量越高，吸附性能越强，凸现了纳米多孔气凝胶材料的优异吸附特性，可选择性的吸附过滤不同分子尺寸的有害物质，同时与纤维或织物的复合解决了气凝胶机械强度差的缺陷；纤维或织物比例越高，复合吸附过滤材料的机械强度就越大，气凝胶的加入提高了纤维吸附过滤材料本身的吸附性能。In the composite adsorption filter material containing porous airgel of the present invention, both the airgel contained therein and the organic or inorganic fiber or fabric have adsorption properties, and the content of the two can be adjusted according to actual application requirements. The higher the airgel content, the stronger the adsorption performance, highlighting the excellent adsorption characteristics of nanoporous airgel materials, which can selectively adsorb and filter harmful substances of different molecular sizes, and at the same time, the combination with fibers or fabrics solves the problem of airgel The defect of poor mechanical strength; the higher the fiber or fabric ratio, the greater the mechanical strength of the composite adsorption filter material, and the addition of airgel improves the adsorption performance of the fiber adsorption filter material itself.
本发明所述的含多孔气凝胶的复合吸附过滤材料，该材料由以正硅酸乙酯为硅源制备的SiO2气凝胶和纤维或织物组成。以正硅酸乙酯为硅源制备的SiO2气凝胶可由下述的方法制得。The composite adsorption filter material containing porous airgel of the present invention is composed of SiO2 airgel and fibers or fabrics prepared by using tetraethyl orthosilicate as silicon source. The SiO 2 aerogel prepared with tetraethyl orthosilicate as the silicon source can be prepared by the following method.
本发明所述的含多孔气凝胶的复合吸附过滤材料，其中SiO2气凝胶和纤维或织物的质量比为0.1～10∶1。The composite adsorption filter material containing porous airgel according to the present invention, wherein the mass ratio of SiO 2 airgel to fiber or fabric is 0.1-10:1.
本发明所述的含多孔气凝胶的复合吸附过滤材料，所述的纤维或织物可以是天然的植物性纤维、动物性纤维、石油化工制品或无机玻璃纤维、陶瓷纤维制品等。In the composite adsorption filter material containing porous airgel of the present invention, the fibers or fabrics may be natural vegetable fibers, animal fibers, petrochemical products, inorganic glass fibers, ceramic fiber products, etc.
本发明所述的含多孔气凝胶的复合吸附过滤材料，材料中气凝胶孔洞率大于80％，孔径尺寸5nm～30nm左右，体积密度50kg/m3～300kg/m3，比表面600～1000m2/g。The composite adsorption filter material containing porous airgel according to the present invention, the airgel porosity in the material is greater than 80%, the pore size is about 5nm-30nm, the bulk density is 50kg/ m3-300kg / m3 , and the specific surface is 600-300nm 1000m 2 /g.
本发明所述的含多孔气凝胶的复合吸附过滤材料的制备方法，其步骤如下：The preparation method of the composite adsorption filter material containing porous airgel of the present invention, its steps are as follows:
a、将正硅酸乙酯、乙醇、水和HF混合后搅拌0.5～5小时，静止存放1～10小时得到SiO2湿凝胶，所用的正硅酸乙酯、乙醇、水和HF的体积比为：1∶3～15∶0.5～1.0∶0.02～0.1；a. Mix ethyl orthosilicate, ethanol, water and HF, stir for 0.5-5 hours, and store it statically for 1-10 hours to obtain SiO2 wet gel. The volume of ethyl orthosilicate, ethanol, water and HF used The ratio is: 1:3~15:0.5~1.0:0.02~0.1;
b、将SiO2湿凝胶和纤维或织物于三甲基氯硅烷与正己烷混合溶液中浸泡修饰18～30小时；b. Soak the SiO2 wet gel and fiber or fabric in a mixed solution of trimethylchlorosilane and n-hexane for 18-30 hours;
c、取出SiO2湿凝胶和纤维或织物后在100～200℃进行热处理，即得到含有SiO2多孔气凝胶的有机或无机纤维或织物。c. After taking out the SiO 2 wet gel and fiber or fabric, perform heat treatment at 100-200° C. to obtain organic or inorganic fiber or fabric containing SiO 2 porous airgel.
本发明所述的含多孔气凝胶的复合吸附过滤材料的制备方法，其中步骤b放入的纤维或织物与SiO2湿凝胶的质量比为0.1～10∶1；所述的纤维或织物可以是天然的植物性纤维、动物性纤维、石油化工制品或无机玻璃纤维、陶瓷纤维制品等；三甲基氯硅烷与正己烷的体积比为1∶5～15。The preparation method of the composite adsorption filter material containing porous airgel of the present invention, wherein the fiber or fabric that step b puts into and SiO The mass ratio of wet gel is 0.1～10:1; Described fiber or fabric It can be natural plant fibers, animal fibers, petrochemical products, inorganic glass fibers, ceramic fiber products, etc.; the volume ratio of trimethylchlorosilane to n-hexane is 1:5-15.
本发明的有益效果：本发明采用常压干燥方法制备纳米多孔气凝胶，在制备多孔气凝胶的同时与纤维或织物复合，省却了许多后期复合的工序和麻烦，制作成本大为降低。用本发明所述的方法制备的复合体中多孔气凝胶的性质不变，分布均匀，比例可调，能很好适用于多种吸附过滤对象。该复合体中的多孔气凝胶与纤维或织物的结合牢固，从根本上克服了多孔气凝胶机械强度低的缺点。Beneficial effects of the present invention: the present invention adopts normal-pressure drying method to prepare nanoporous airgel, and composites with fiber or fabric at the same time of preparing porous airgel, which saves many post-compositing procedures and troubles, and greatly reduces production cost. The properties of the porous airgel in the complex prepared by the method of the invention are unchanged, the distribution is uniform, and the ratio can be adjusted, which is well applicable to various adsorption and filtration objects. The porous airgel in the composite is firmly combined with the fiber or fabric, which fundamentally overcomes the shortcoming of the low mechanical strength of the porous airgel.
具体实施方式Detailed ways
实施例1Example 1
将100ml正硅酸乙酯、1500ml无水乙醇、60ml蒸馏水和2mlHF均匀混合后搅拌0.5hr，静止存放10hr，得到SiO2湿凝胶。将SiO2湿凝胶捣碎浸泡于体积比为1∶8的三甲基氯硅烷与正己烷混合溶液中，常温下浸泡做表面修饰，并将木质纤维素一并放入，放入纤维的总量与SiO2多孔气凝胶质量比为1∶10。24小时后取出，待表面干燥后放入烘箱加温至200℃进行热处理，即得到含有SiO2多孔气凝胶的有机纤维，即含多孔气凝胶的复合吸附过滤材料。Mix 100ml tetraethyl orthosilicate, 1500ml absolute ethanol, 60ml distilled water and 2mlHF evenly, stir for 0.5hr, and store it statically for 10hr to obtain SiO2 wet gel. The SiO 2 wet gel was smashed and soaked in a mixed solution of trimethylchlorosilane and n-hexane with a volume ratio of 1:8, soaked at room temperature for surface modification, and put lignocellulose together, and put it in the fiber The mass ratio of the total amount to the SiO2 porous airgel is 1:10. Take it out after 24 hours, put it into an oven and heat it to 200°C for heat treatment after the surface is dry, and then obtain organic fibers containing SiO2 porous airgel, namely Composite adsorption filter material containing porous airgel.
经ASAP-2000型物理吸附仪检测，材料中气凝胶孔洞率92％，孔径尺寸20nm，体积密度120kg/m3，比表面积800m2/g。该气凝胶复合吸附过滤材料可用于吸附四氯化碳、甲醛、甲苯等有毒气体，吸附过滤性能很好。As detected by ASAP-2000 physical adsorption instrument, the airgel porosity in the material is 92%, the pore size is 20nm, the bulk density is 120kg/m 3 , and the specific surface area is 800m 2 /g. The airgel composite adsorption filter material can be used for adsorption of carbon tetrachloride, formaldehyde, toluene and other toxic gases, and has good adsorption and filtration performance.
实施例2Example 2
将100ml正硅酸乙酯、1000ml无水乙醇、100ml蒸馏水和10mlHF均匀混合后搅拌2小时，静止存放1小时，得到SiO2湿凝胶。将SiO2湿凝胶捣碎浸泡于体积比为1∶15的三甲基氯硅烷与正己烷混合溶液中，常温下浸泡作表面修饰，同时还放入硅酸钙浆料、金红石型钛白粉、陶瓷纤维、玻璃纤维、多孔水泥，其加入量与SiO2湿凝胶按质量比分别为10∶5∶1∶1∶0.5∶100。30小时后取出，待表面干燥后放入烘箱加温至100℃进行热处理，再压制成块体，即得到疏水型二氧化硅气凝胶复合材料块体。Mix 100ml tetraethyl orthosilicate, 1000ml absolute ethanol, 100ml distilled water and 10ml HF evenly, stir for 2 hours, and store it statically for 1 hour to obtain SiO 2 wet gel. The SiO 2 wet gel is crushed and soaked in a mixed solution of trimethylchlorosilane and n-hexane with a volume ratio of 1:15, soaked at room temperature for surface modification, and calcium silicate slurry and rutile titanium dioxide are also added at the same time , ceramic fiber, glass fiber, porous cement, and its addition amount is 10:5:1:1:0.5:100 by mass ratio with SiO2 wet gel respectively. Take it out after 30 hours, put it into the oven to heat after the surface is dry Heat treatment at 100°C, and then press into a block to obtain a block of hydrophobic silica airgel composite material.
经ASAP-2000型物理吸附仪检测，材料中气凝胶孔洞率90％，孔径尺寸10nm左右，体积密度150kg/m3，比表面积600m2/g。该气凝胶复合吸附过滤材料可用于吸附亚甲基蓝，乙醛、三氯甲烷等有毒物质，吸附过滤性能很好。As detected by ASAP-2000 physical adsorption instrument, the airgel porosity in the material is 90%, the pore size is about 10nm, the bulk density is 150kg/m 3 , and the specific surface area is 600m 2 /g. The airgel composite adsorption filter material can be used for adsorption of methylene blue, acetaldehyde, chloroform and other toxic substances, and has good adsorption and filtration performance.
实施例3Example 3
将100ml正硅酸乙酯、300ml无水乙醇、50ml蒸馏水和6mlHF均匀混合后搅拌5hr，静止存放3小时，得到SiO2湿凝胶。将SiO2湿凝胶捣碎浸泡于体积比为1∶5的三甲基氯硅烷与正己烷混合溶液中，常温下浸泡作表面修饰，同时还放入陶瓷纤维，其总加入量与SiO2湿凝胶按质量比为10∶1。18小时后取出，待表面干燥后放入烘箱加温至150℃进行热处理，再压制成块体，即得到疏水型含多孔气凝胶的复合吸附过滤材料。Mix 100ml tetraethyl orthosilicate, 300ml absolute ethanol, 50ml distilled water and 6ml HF evenly, stir for 5hr, and store it statically for 3 hours to obtain SiO 2 wet gel. The SiO 2 wet gel is crushed and soaked in a mixed solution of trimethylchlorosilane and n-hexane with a volume ratio of 1:5, soaked at room temperature for surface modification, and ceramic fibers are also added at the same time, and the total amount added is the same as that of SiO 2 The mass ratio of the wet gel is 10:1. Take it out after 18 hours. After the surface is dry, put it in an oven and heat it to 150°C for heat treatment, and then press it into a block to obtain a hydrophobic composite adsorption filter with porous airgel. Material.
经ASAP-2000型物理吸附仪检测，材料中气凝胶孔洞率80％，孔径尺寸5nm左右，体积密度200kg/m3，比表面积600m2/g。该气凝胶复合吸附过滤材料可用于吸附水中苯酚、吡啶等有毒物质，吸附过滤性能很好。As detected by ASAP-2000 physical adsorption instrument, the airgel porosity in the material is 80%, the pore size is about 5nm, the bulk density is 200kg/m 3 , and the specific surface area is 600m 2 /g. The airgel composite adsorption filter material can be used to absorb toxic substances such as phenol and pyridine in water, and has good adsorption and filter performance.
由以上具体实施方式可知，本发明采用常压干燥方法制备纳米多孔气凝胶，在制备多孔气凝胶的同时与纤维或织物复合，省却了许多后期复合的工序和麻烦，制作成本大为降低。用本发明所述的方法制备的复合体中纤维或织物与SiO2湿凝胶比例可调，能适用于多种吸附过滤对象，应用范围广泛。It can be seen from the above specific implementation methods that the present invention adopts the normal pressure drying method to prepare nanoporous airgel, and composites with fibers or fabrics while preparing porous airgel, which saves many later composite procedures and troubles, and greatly reduces the production cost . The proportion of fiber or fabric and SiO2 wet gel in the complex prepared by the method of the invention can be adjusted, can be applied to various adsorption and filtration objects, and has a wide range of applications.
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