高等学校化学学报 ›› 2009, Vol. 30 ›› Issue (7): 1279.

• 研究论文 • 上一篇    下一篇

多孔SiC陶瓷微孔道内合成Silicalite-2分子筛膜

罗民1,2, 梁军2, 房俊卓1, 王政1   

  1. 1. 宁夏大学能源化工国家重点实验室,
    2. 化学化工学院, 银川 750021
  • 收稿日期:2008-10-07 出版日期:2009-07-10 发布日期:2009-07-10
  • 通讯作者: 罗民, 男, 博士, 副教授, 主要从事多孔功能材料的设计和优化研究. E-mail: luominjy@nxu.edu.cn
  • 基金资助:

    国家“九七三”计划(批准号: 2007CB216402), 教育部科学技术研究重点项目(批准号: 203143)和宁夏高等学校科研项目资助.

Growth of Silicalite-2 Zeolite Film in Microchannels of Biomorphic Porous SiC Ceramics

LUO Min1,2*, LIANG Jun2, FANG Jun-Zhuo1, WANG Zheng1   

  1. 1. Key Laboratory of Energy Resources and Chemical Engineering,
    2. Department of Chemical Science and Engineering, Ningxia University, Yinchuan 750021, China
  • Received:2008-10-07 Online:2009-07-10 Published:2009-07-10
  • Contact: LUO Min. E-mail: luominjy@nxu.edu.cn
  • Supported by:

    国家“九七三”计划(批准号: 2007CB216402), 教育部科学技术研究重点项目(批准号: 203143)和宁夏高等学校科研项目资助.

摘要:

榉木经高温热解转化为生物碳模板, 通过液相渗硅反应工艺制备了保持木材微观结构的多孔SiC陶瓷. 在生物形态多孔SiC陶瓷载体上采用原位沉积晶种-二次生长法在其微孔道内壁形成了一层5 μm厚的Silicalite-2分子筛膜. 利用XRD, SEM和BET对复合材料的相组成、微观结构和比表面积进行了表征, 研究了水热晶化温度对原位沉积晶种和二次生长成膜的影响. 经原位沉积(120 ℃, 36 h)晶种涂层后在载体孔道表面形成了一层球形颗粒堆积的连续晶种层, 经170 ℃, 36 h的二次生长, 晶种不断长大并交织生长形成连续致密单层分子筛膜. 在多孔SiC陶瓷微孔道中沿垂直于载体表面方向形成了一层对齐排列的Silicalite-2棒状晶体, 颗粒生长主要沿晶体的最长轴[101]方向进行. Silicalite-2/SiC复合孔结构材料的微孔体积为0.013 cm3/g, BET比表面积为43.2 m2/g, 而相应的分子筛负载量为9.5%.

关键词: 生物形态多孔SiC陶瓷; 分子筛膜; Silicalite-2; 原位沉积晶种-二次水热生长

Abstract:

Aligned Silicate-2 zeolite membrane was synthesized by in situ seeding and secondary crystal growth in microchannels of biomorphic porous SiC ceramics support. The Silicate-2/SiC composite materials were characterized by XRD, SEM and BET. The effects of synthesis temperature and seed surface pre-treatment of the beech-derived SiC monolith were studied. The results show that a homogeneous coverage of 5 μm thick zeolite membrane within the pores channel of SiC monolith by Silicate-2 crystals was reached after in situ seeding at 120 ℃ for 36 h with a following hydrothermal treatment at 170 ℃ for 36 h. The film oriented with [101] axis perpendicular to the substrate surface. The structure composites exhibit a hierarchical pore structure with a BET specific surface area of 43.2 m2/g and microporous volume of 0.013 cm3/g. The weight percent of Silicate-2 in the final Silicate-2/SiC composites is about 9.5% after a coating procedure.

Key words: Biomorphous porous SiC ceramics; Zeolite membrane; Silicalite-2; In situ seed and secondary crystal growth

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