文章摘要
周永贤,陈伟,王鹏飞,张毅民.13X分子筛膜制备及其在低碳烯烃净化中的应用[J].精细化工,2018,35(12):
13X分子筛膜制备及其在低碳烯烃净化中的应用
Preparation of 13X Molecular Sieve Membranes and Its Application in Light Olefins Deeply Purification
投稿时间:2018-03-02  修订日期:2018-05-03
DOI:
中文关键词: 13X分子筛膜  多孔α-Al2O3陶瓷管  密实连续  低碳烯烃深度净化  含氧化物
英文关键词: 13X membranes  porous α-Al2O3 tube  dense and continuous  light olefins deeply purification  oxygenated compounds
基金项目:
作者单位E-mail
周永贤 天津大学 zhouyongxian@126.com 
陈伟 上海化工研究院有限公司  
王鹏飞 上海化工研究院有限公司  
张毅民 天津大学 zhangym@tju.edu.cn 
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中文摘要:
      以多孔α-Al2O3陶瓷管为支撑体,3-氨丙基三乙氧基硅烷(APTES)为表面改性剂,运用真空溶胶预涂覆以及水热晶化的方法,在α-Al2O3陶瓷管表面制备出了密实连续均匀且无任何孔或裂纹存在的13X分子筛膜层。重点研究了表面改性剂浓度、水热晶化次数对分子筛膜层的影响。结果表明,当APTES浓度为46 mg/ml,水热晶化次数为2次时,所制备的13X分子筛膜层最佳。该13X分子筛膜能将氮气和乙烯气体中初始含量为20?10-6 mol/mol的二甲醚、甲醇、丙醛三种含氧化物杂质脱除至1?10-6 mol/mol以下。与颗粒状13X分子筛相比,该13X分子筛膜展现出更好的含氧化物深度脱除性能。在氮气为原料气时,该13X分子筛膜对二甲醚、甲醇、丙醛的穿透时间分别为16 h、44.7 h和94 h。在乙烯为原料气时,对二甲醚、甲醇、丙醛的穿透时间分别为25.2 h、102 h和178 h。
英文摘要:
      In this study, we successfully fabricated dense and thin 13X molecular sieve membranes without any cracks, pinholes or other defects on porous α-Al2O3 tube by combination of 3-aminopropyl triethoxy silane (APTES) surface modification, vacuum pre-coating sol technology and hydrothermal crystallization method. The effects of APTES concentration and hydrothermal crystallization number on 13X molecular sieve layers were studied emphatically. The results demonstrated that the best 13X molecular sieve membranes with a thickness of about 10~15 μm could be obtained with 46 mg/ml of APTES surface treatment and 2 times of hydrothermal crystallization. The purification results indicated that the above 13X molecular sieve membranes could deeply purify the trace amount of dimethyl ether, methanol and propanal impurities to below 1?10-6 mol/mol from gaseous olefins at the initial concentration of 20?10-6 mol/mol under room temperature, exhibiting much more excellent purification performance than that of granular 13X molecular sieve adsorbents. In particular, the breakthrough times of 13X molecular sieve membranes for dimethyl ether, methanol and propanal were 16 h, 44.7 h, 94 h in N2 system, and 25.2 h, 102 h, 178 h in C2H4 system.
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