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小野百合

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[求助] Synthesis of ZSM-5 structures via template-free sol–gel method

Hierarchical porous materials with ZSM-5 structures were synthesized by a three-step procedure.
     The first step consists of the preparation of ZSM-5 precursor sol. In a typical synthesis, 25.4 g of 20% aqueous solution of TPAOH was added to the mixture of 20.8 g of TEOS and 0.4 g of Al(i-OPr)3 under vigorous stirring at 273K to obtain a turbid solution with molar composition of 1.0TEOS: 0.02Al(i-OPr)3: 0.25TPAOH: 11.3H2O. Clear ZSM-5 precursor sol containing a little floccule was obtained by stirring the turbid solution at 323K for 48 h.
     In the second step, the ZSM-5 precursor sol filtrated floccule was dried at 303K in a vacuum box retaining the vacuum value of 6.65 kPa until it became xerogel. Thesilica content in the xerogel was about 7.7*10-3mol/g.
    The third step involves the recrystallization of the xerogel. The mixture of xerogel and water (1Si: 150 water, molar ratio) was transferred into Teflon-lined stainless steel autoclaves and carried out hydrothermal synthesis at a certain temperature for 24 h. Finally, the solid products were filtered, washed, dried at 303K in a vacuum box and calcined at 823K in air for 6 h. The obtained hierarchical porous materials were named as HPM-X, where X indicates the temperature of recrystallization. For comparison, the direct-calcined xerogel (DCX) was also prepared.
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jiangguofeng

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RXMCDM: 金币+1 2014-05-21 11:29:16
小野百合: 金币+5, 翻译EPI+1, ★★★很有帮助 2014-05-21 15:21:04
小野百合(RXMCDM代发): 金币+5 2014-05-22 00:25:12
无模板溶胶-凝胶法合成ZSM-5结构

通过一种三步方法合成具有ZSM - 5结构的分层多孔材料。
     第一步制备ZSM -5前体溶胶。在一种曲型的合成方法当中,强烈搅拌下于273K温度中,将25.4克20%四丙基氢氧化铵水溶液加到20.8克正硅酸乙酯和0.4克三异丙氧基铝的混合物中,得到一种浑浊液,其摩尔组成为1.0正硅酸乙酯:0.02三异丙氧基铝:0.25四丙基氢氧化铵:11.3 H2O。于323K温度中搅拌这种浑浊液48小时,得到含有少量?occule的透明的ZSM-5前体溶胶。
    第二步,于一个保持6.65 kPa真空度的真空箱中,于303K温度干燥这种ZSM - 5前体溶胶?ltrated ?occule直至成为干凝胶。干凝胶中的含硅量为大约7.7×10 - 3mol/克。  第三步包括干凝胶的再结晶。将这种干凝胶和水(1 Si : 150 水,摩尔比)的混合物移至Te?on -衬里的白钢高压釜中,于一定温度进行热液合成24小时。 最后,固体产物经过滤、洗涤、于真空箱中303k温度干燥以及于823K温度在大气环境下焙烧6小时。得到的分层多孔材料命名为HPM - X,其中X表示再结晶温度。作为对比,也制备了直接焙烧干凝胶(DCX)。
2楼2014-05-21 11:16:53
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