CN114790004A - 一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法 - Google Patents
一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法 Download PDFInfo
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Abstract
本发明属于新材料的制备领域,涉及一种用无机金属盐制备耐高温SiO2‑AxOy气凝胶的方法。本方法以水玻璃为硅源、水为溶剂,水玻璃水解制备氧化硅溶胶,以金属无机盐水解形成无机金属氧化物溶胶,两种溶胶混合,经老化、溶剂置换、表面改性和干燥得到一种用耐高温SiO2‑AxOy气凝胶。本发明制备的耐高温SiO2‑AxOy气凝胶具有较高的比表面积、优异的耐高温性能而且成本低,可实现工业化生产。
Description
技术领域
本发明属于新材料的制备领域,具体涉及一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法。
背景技术
氧化硅气凝胶是一种由纳米颗粒聚集而成的轻质多孔纳米材料,所具备的高孔隙率可降低热传导,使得氧化硅气凝胶具有优异的保温隔热性能。氧化硅气凝胶普遍存在成本高,耐高温性能差等问题,这些问题极大地限制了氧化硅气凝胶的规模化生产和应用。因此需提高气凝胶的耐高温性能,同时降低生产成本。水玻璃可通过水解聚合反应得到氧化硅溶胶,具有较低的价格,是一种很好的硅源,金属无机盐可通过水解形成金属氧化物溶胶,将氧化硅溶胶与无机金属氧化物溶胶混合凝胶,即可制得耐高温SiO2-AxOy气凝胶。
发明内容
为了改进现有氧化硅气凝胶材料成本高、耐高温性能差等问题,本发明提出了一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法,选用优质廉价的水玻璃为硅源,制备氧化硅溶胶,同时以金属无机盐水解制备无机金属氧化物溶胶,两种溶胶混合凝胶制备耐高温SiO2-AxOy气凝胶。本发明解决了气凝胶材料成本高、耐高温性能差等问题,同时反应条件简单可控,可适用于工业化生产。
本发明的技术方案为:一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法,其步骤如下:
(1)按以下重量份记:将水玻璃5~10份、水35~75份混合搅拌0.5~1.5h,加入酸调节混合溶液的pH为1~2,混合搅拌0.5~1.5h得到氧化硅溶胶;
(2)按以下重量份记:将金属无机盐5~10份、水40~80份、酸0.1~0.5份混合搅拌1.5~3.5h,形成澄清透明的无机金属氧化物溶胶;
(3)将步骤(1)得到的氧化硅溶胶与步骤(2)得到的无机金属氧化物溶胶按1~3:1的体积比混合搅拌0.5~1.5h得到混合溶胶;
(4)将步骤(3)得到的混合溶胶加入凝胶促进剂50~150重量份,混合搅拌0.1~0.5h,得到混合液;
(5)将步骤(4)得到的混合液在20~50℃下凝胶化得到湿凝胶;
(6)将步骤(5)得到的湿凝胶在20~70℃下陈化6~72h;
(7)步骤(6)得到的湿凝胶放入有机溶剂中进行溶剂置换4~6次,每次3~6h;
(8)步骤(7)得到的湿凝胶放入疏水改性液中进行疏水改性,改性时间1~24h;
(9)将步骤(8)中的湿凝胶进行超临界干燥即可制得耐高温SiO2-AxOy气凝胶。
优选步骤(1)中所述的酸为冰醋酸、草酸、盐酸、硝酸或硫酸中的一种。
优选步骤(2)中所述的金属无机盐为氯化铝、硝酸铝、氯化锆、氯化钛或氯化钇中的一种。优选步骤(2)中所述的酸为草酸或冰醋酸。
优选步骤(4)中所述的凝胶促进剂为尿素、氨水或环氧丙烷。
优选步骤(7)中所述的有机溶剂为甲醇、乙醇、丙酮或正己烷。
优选步骤(8)中所述的疏水改性液为疏水改性剂与有机溶剂的混合液,其中疏水改性剂与有机溶剂的重量比为1:(10-100);所述的有机溶剂与步骤(7)中的有机溶剂一致。
优选步骤(8)中所述的疏水改性剂为三甲基氯硅烷、甲基甲氧基硅烷、甲基乙氧基硅烷或六甲基二硅氮烷。
本发明所制备得到的SiO2-AxOy气凝胶的密度为0.030~0.15g/cm3,比表面积为600~900m2/g,疏水角为125°~135°,1000℃热处理0.5h后比表面积衰减40%~60%。
有益效果:
本发明选用优质价廉的水玻璃为硅源制备氧化硅气凝胶溶液,同时以金属无机盐水解制备无机金属氧化物溶胶,两种溶胶混合凝胶制备耐高温SiO2-AxOy气凝胶,制备成本低,操作简单。水玻璃、无机金属盐与水混合后无毒、无味,对人体和环境无影响。
本发明在制备过程中通过酸调节溶液的pH,再通过凝胶促进剂缩短凝胶时间,使其迅速发生缩聚反应制得湿凝胶,反应条件方便可控,周期短。
附图说明
图1为实例1制得的耐高温SiO2-AxOy气凝胶样品图片。
具体实施方式
以下实施例所述的份均为重量份。
实例1
5份水玻璃、35份水混合搅拌0.5h,加入冰醋酸调节溶液pH为1混合搅拌0.5h得到氧化硅溶胶。5份氯化铝、40份水、0.1份冰醋酸混合搅拌1.5h,得到氧化铝溶胶。将氧化硅溶胶与氧化铝溶胶按3:1体积比混合搅拌1.5h,加入78份环氧丙烷混合搅拌0.1h,在25℃下凝胶化得到湿凝胶。将湿凝胶在20℃的条件下陈化72h,再放入乙醇溶液中进行溶剂置换,置换6次,每次3h。将溶剂置换后的湿凝胶放入1份三甲基氯硅烷与100份乙醇溶液的混合液中进行疏水改性,改性时间为12h。最后将湿凝胶进行CO2超临界干燥,即可得到完整块状耐高温SiO2-Al2O3气凝胶。制备的SiO2-Al2O3气凝胶,其密度0.030g/cm3,比表面积900m2/g,疏水角135°,1000℃热处理0.5h后比表面积衰减40%。
实例2
10份水玻璃、75份水混合搅拌1.5h,加入草酸调节溶液pH为2混合搅拌1.5h得到氧化硅溶胶。8份硝酸铝、70份水、0.5份冰醋酸混合搅拌3.5h得到氧化铝溶胶。将氧化硅溶胶与氧化铝溶胶按1:1比例混合搅拌0.5h,加入50份氨水混合搅拌0.5h,在50℃下凝胶化得到湿凝胶。将湿凝胶放入70℃的烘箱中陈化6h,再加入甲醇溶液进行溶剂置换,置换4次,每次6h。将溶剂置换后的湿凝胶放入1份甲基三甲氧基硅烷与10份甲醇溶液的混合液中进行疏水改性,改性时间为1h,最后将湿凝胶进行CO2超临界干燥,即可得到块状耐高温SiO2-Al2O3气凝胶。制备的SiO2-Al2O3气凝胶,其密度0.038g/cm3,比表面积786m2/g,疏水角125°,1000℃热处理0.5h后比表面积衰减45%。
实例3
8份水玻璃、60份水混合搅拌0.8h,加入盐酸调节溶液pH为1.5混合搅拌1h得到氧化硅溶胶。10份氯化锆、80份水、0.3份草酸混合搅拌1.5h得到氧化锆溶胶。将氧化硅溶胶与氧化锆溶胶按2:1比例混合搅拌1h,加入150份尿素混合搅拌0.3h,20℃下凝胶化得到湿凝胶。将湿凝胶放入50℃的烘箱中陈化12h,再加入丙酮溶液进行溶剂置换,置换6次,每次3h。将溶剂置换后的湿凝胶放入1份甲基三乙氧基硅烷与90份丙酮溶液的混合液中进行疏水改性,改性时间为12h,最后将湿凝胶进行CO2超临界干燥,即可得到块状耐高温SiO2-ZrO2气凝胶。制备的SiO2-ZrO2气凝胶,其密度0.15g/cm3,比表面积600m2/g,疏水角129°,1000℃热处理0.5h后比表面积衰减50%。
实例4
6份水玻璃、60份水混合搅拌0.5h,加入硫酸调节溶液pH为2混合搅拌1h得到氧化硅溶胶。8份氯化钛、60份水、0.2份草酸混合搅拌2.5h得到氧化钛溶胶。将氧化硅溶胶与氧化钛溶胶按3:1比例混合搅拌0.8h,加入110份环氧丙烷混合搅拌0.5h,在30℃下凝胶化得到湿凝胶。将湿凝胶放入50℃的烘箱中陈化6h,再加入正己烷溶液进行溶剂置换,置换6次,每次6h。将溶剂置换后的湿凝胶放入1份甲基三乙氧基硅烷与90份正己烷溶液的混合液中进行疏水改性,改性时间为24h,最后将湿凝胶进行CO2超临界干燥,即可得到块状耐高温SiO2-TiO2气凝胶。制备的SiO2-TiO2气凝胶,其密度0.050g/cm3,比表面积680m2/g,疏水角130°,1000℃热处理0.5h后比表面积衰减60%。
实例5
5份水玻璃、60份水混合搅拌1.5h,加入盐酸调节溶液pH为2混合搅拌1.5h得到氧化硅溶胶。6份氯化钇、70份水、0.4份冰醋酸混合搅拌1h得到氧化钇溶胶。将氧化硅溶胶与氧化钇溶胶3:1比例混合搅拌1.5h,加入125份网络形成剂混合搅拌0.5h,在35℃下凝胶化得到湿凝胶。将湿凝胶放入45℃的烘箱中陈化24h,再加入乙醇溶液进行溶剂置换,置换6次,每次6h。将溶剂置换后的湿凝胶放入1份六甲基二硅氮烷与100份乙醇溶液的混合液中进行疏水改性,改性时间为24h,最后将湿凝胶进行CO2超临界干燥,即可得到块状耐高温SiO2-Yi2O3气凝胶。制备的SiO2-Yi2O3气凝胶,其密度0.036g/cm3,比表面积720m2/g,疏水角133°,1000℃热处理0.5h后比表面积衰减55%。
Claims (9)
1.一种用金属无机盐制备耐高温SiO2-AxOy气凝胶的方法,其步骤如下:
(1)按以下重量份记:将水玻璃5~10份、水35~75份混合搅拌0.5~1.5h,加入酸调节混合溶液的pH为1~2,混合搅拌0.5~1.5h得到氧化硅溶胶;
(2)按以下重量份记:将金属无机盐5~10份、水40~80份、酸0.1~0.5份混合搅拌1.5~3.5h,形成澄清透明的无机金属氧化物溶胶;
(3)将步骤(1)得到的氧化硅溶胶与步骤(2)得到的无机金属氧化物溶胶按1~3:1的体积比混合搅拌0.5~1.5h得到混合溶胶;
(4)将步骤(3)得到的混合溶胶加入凝胶促进剂50~150重量份,混合搅拌0.1~0.5h,得到混合液;
(5)将步骤(4)得到的混合液在20~50℃下凝胶化得到湿凝胶;
(6)将步骤(5)得到的湿凝胶在20~70℃下陈化6~72h;
(7)步骤(6)得到的湿凝胶放入有机溶剂中进行溶剂置换4~6次,每次3~6h;
(8)步骤(7)得到的湿凝胶放入疏水改性液中进行疏水改性,改性时间1~24h;
(9)将步骤(8)中的湿凝胶进行超临界干燥即可制得耐高温SiO2-AxOy气凝胶。
2.根据权利要求1所述的方法,其特征在于步骤(1)中所述的酸为冰醋酸、草酸、盐酸、硝酸或硫酸中的一种。
3.根据权利要求1所述的方法,其特征在于步骤(2)中所述的金属无机盐为氯化铝、硝酸铝、氯化锆、氯化钛或氯化钇中的一种。
4.根据权利要求1所述的方法,其特征在于步骤(2)中所述的酸为草酸或冰醋酸。
5.根据权利要求1所述的方法,其特征在于步骤(4)中所述的凝胶促进剂为尿素、氨水或环氧丙烷。
6.根据权利要求1所述的方法,其特征在于步骤(7)中所述的有机溶剂为甲醇、乙醇、丙酮或正己烷。
7.根据权利要求1所述的方法,其特征在于步骤(8)中所述的疏水改性液为疏水改性剂与有机溶剂的混合液,其中疏水改性剂与有机溶剂的重量比为1:(10-100);所述的有机溶剂与步骤(7)中的有机溶剂一致。
8.根据权利要求1所述的方法,其特征在于步骤(8)中所述的疏水改性剂为三甲基氯硅烷、甲基甲氧基硅烷、甲基乙氧基硅烷或六甲基二硅氮烷。
9.根据权利要求1所述的方法,其特征在于所制备得到的SiO2-AxOy气凝胶的密度为0.030~0.15g/cm3,比表面积为600~900m2/g,疏水角为125°~135°,1000℃热处理0.5h后比表面积衰减40%~60%。
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