WO2022078362A1 - 一种间二甲苯吸附剂及其制备方法 - Google Patents
一种间二甲苯吸附剂及其制备方法 Download PDFInfo
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- WO2022078362A1 WO2022078362A1 PCT/CN2021/123445 CN2021123445W WO2022078362A1 WO 2022078362 A1 WO2022078362 A1 WO 2022078362A1 CN 2021123445 W CN2021123445 W CN 2021123445W WO 2022078362 A1 WO2022078362 A1 WO 2022078362A1
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- molecular sieve
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Abstract
Description
Claims (21)
- 一种间二甲苯吸附剂,包括94~99.9质量%的Y分子筛和0.1~6质量%的基质,所述Y分子筛由非转晶Y分子筛和转晶生成的Y分子筛组成,所述非转晶Y分子筛为介孔纳米Y分子筛,所述介孔纳米Y分子筛的晶粒粒径为20~450纳米,含有两种介孔孔道,最可几孔直径分别为5~20纳米和25~50纳米。
- 按照权利要求1所述的吸附剂,包括98~99.9质量%的Y分子筛和0.1~2质量%的基质。
- 按照权利要求1所述的吸附剂,包括84~93质量%的非转晶Y分子筛、1~15.9质量%的转晶生成的Y分子筛和0.1~6质量%的基质。
- 按照权利要求1-3任一项所述的吸附剂,其特征在于所述的吸附剂包括84~93质量%的非转晶Y分子筛、5~15.9质量%的转晶生成的Y分子筛和0.1~2质量%的基质。
- 按照权利要求1-4任一项所述的吸附剂,其特征在于所述介孔纳米Y分子筛为纳米级Y分子筛晶粒自聚体,自聚体粒径为0.5~1.5微米,自聚体中纳米级Y分子筛晶粒粒径为20~400纳米。
- 按照权利要求1-4任一项所述的吸附剂,其特征在于所述介孔纳米Y分子筛的SiO 2/Al 2O 3摩尔比为4.0~5.5。
- 按照权利要求1-4任一项所述的吸附剂,其特征在于所述介孔纳米Y分子筛的比表面积为740~1000m 2/g,总孔体积为0.40~0.65cm 3/g,介孔孔体积为0.08~0.35cm 3/g。
- 按照权利要求1-4任一项所述的吸附剂,其特征在于所述介孔纳米Y分子筛的最可几孔径分别为10~20纳米和30~50纳米。
- 一种权利要求1-8任一项所述吸附剂的制备方法,包括如下步骤:(1)将非转晶NaY分子筛、高岭土矿物、硅源和成型助剂混合均匀,滚球成型制成小球,干燥后于530~600℃焙烧,所述非转晶NaY分子筛与高岭土矿物的质量比为85~94∶6~15,加入的硅源中所含二氧化硅与高岭土矿物的质量比为0.1~3.6;(2)将(1)步焙烧后所得小球用氢氧化钠或氢氧化钠与水玻璃的 混合溶液于85~100℃进行原位晶化处理,使其中的高岭土矿物原位晶化为Y分子筛,然后水洗、干燥。
- 按照权利要求9所述的方法,其特征在于(1)步所述的高岭土矿物选自高岭石、地开石、珍珠石、耐火石、埃洛石或它们的混合物。
- 按照权利要求9所述的方法,其特征在于(1)步所述的成型助剂选自木质素、田菁粉、干淀粉、羧甲基纤维素和活性碳中的至少一种。
- 按照权利要求9所述的方法,其特征在于(1)步中所述的硅源选自正硅酸乙酯、硅溶胶、水玻璃、硅酸钠、硅胶和白炭黑中的一种或几种,加入的硅源中所含二氧化硅与高岭土矿物的质量比为0.2~3.0。
- 按照权利要求9所述的方法,其特征在于(2)步中原位晶化处理的液/固比为1.5~5.0升/千克。
- 按照权利要求9所述的方法,其特征在于(2)步原位晶化处理使用氢氧化钠溶液时,其中氢氧根离子的浓度为0.1~3.0摩尔/升;当原位晶化处理使用氢氧化钠和水玻璃混合溶液时,其中氧化钠含量为2~10质量%,二氧化硅含量为1~6质量%。
- 按照权利要求9所述的方法,其特征在于(1)步所述的非转晶NaY分子筛的制备方法,包括如下步骤:(I)取0~5℃的硅源、铝源,加入氢氧化钠、水混合均匀形成分子筛合成体系,其中各物料的摩尔比为:SiO 2/Al 2O 3=5.5~9.5、Na 2O/SiO 2=0.1~0.3、H 2O/SiO 2=5~25,合成体系的温度为1~8℃,(II)将(I)步的分子筛合成体系于20~40℃静态老化10~48小时,再于90~150℃静态晶化2~10小时,搅拌2~10分钟,继续静态晶化11~20小时,将所得固体洗涤、干燥。
- 按照权利要求15所述的方法,其特征在于(I)步所述分子筛合成体系中各物料的摩尔比为:SiO 2/Al 2O 3=7~9、Na 2O/SiO 2=0.1~0.25、H 2O/SiO 2=8~20。
- 按照权利要求15所述的方法,其特征在于(II)步将分子筛合成体系于20~40℃静态老化15~30小时,再于90~120℃静态晶化4~9小时,搅拌2~10分钟,继续静态晶化11~15小时。
- 按照权利要求15所述的方法,其特征在于(I)步所述的铝源选自低碱度偏铝酸钠溶液、氧化铝、氢氧化铝、硫酸铝溶液、氯化铝、硝酸铝和铝酸钠中的一种或几种。
- 按照权利要求15所述的方法,其特征在于低碱度偏铝酸钠溶液中Al 2O 3含量为17~28质量%,Na 2O含量为19~30质量%。
- 按照权利要求15所述的方法,其特征在于所述的硅源选自硅溶胶或水玻璃。
- 按照权利要求20所述的方法,其特征在于所述水玻璃中SiO 2含量为25~38质量%,Na 2O含量为9~15质量%。
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CN1354134A (zh) * | 2001-10-19 | 2002-06-19 | 中国石油化工股份有限公司 | 一种小晶粒y型分子筛的合成方法 |
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CN106927478A (zh) * | 2015-12-30 | 2017-07-07 | 中国石油化工股份有限公司 | 一种y型分子筛的改性方法 |
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