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briefshao银虫 (初入文坛)
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求教！NaY型zeolite和BET的孔隙率问题！
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不是化学的背景，现在在做FAU NaY type的zeolite，问题多多，求教各位牛人。 1. 我们用micromeritcs公司的ASAP2020做BET，如何计算porosity（孔隙率）。 2. 做seeding粉和做膜的时候，炉子是pre-heated还是把东西放进去后一起升温，到了时间是要炉冷、水冷还是... 3. 做的粉（碱性很强）是要洗的吧，洗到什么时候为好。 4. 配制溶液时原料的先后顺序重要吗？ 5. dip-coating的技巧？ 6. 文献里的时间都是要很准确吗？ 非常感谢各位！！！ 附： 老板指定参考的做法： 文献：Synthesis of Defect-Free FAU-Type Zeolite Membranes and Separation for Dry and Moist CO2/N2 Mixtures. Ind. Eng. Chem. Res. 2005, 44, 937-944 Faujasite zeolite membranes were prepared by a seeding and secondary growth approach. Disc-shaped porous a-Al2O3 substrates were seeded with NaY zeolite crystals with a size of 1-1.5 um. The NaY seed particles were synthesized from an aluminosilicate gel with a molar composition of 12.8:1:17:675 SiO2/Al2O3/Na2O/H2O. The temperature and time for hydrothermal synthesis of the seed particles were 90 °C and 12 h. The substrates were seeded by dip coating with zeolite suspensions. The zeolite seed suspension for dip coating was prepared by dispersing 0.1 g of the synthesized NaY powders in 25 mL of deionized water. The suspension was adjusted to pH 3-4 by adding a 1.0 M HNO3 solution. The suspension was stirred rigorously for 24 h before use. After dip coating, the coated disks were dried at 60 °C in air for 24 h. The aluminosilicate gel used for secondary growth had a composition of 10.7:1:18.8:850 SiO2/Al2O3/Na2O/H2O. The synthesis gel was prepared by mixing water glass (27% SiO2 + 14% NaOH; Aldrich), sodium aluminate [50-56% Al + 40-45% Na (Fe < 0.05%); Riedel-deHaen], and sodium hydroxide (99.99%; Aldrich). The gel was rigorously stirred for 12 h and poured into an autoclave, where a substrate was mounted horizontally on a stand with its seeded side facing downward. Hydrothermal crystallization was carried out at 100 °C in the closed autoclave for 4-6 h. The synthesized membranes were washed with deionized water and then dried at 60 °C in air for at least 24 h before any tests or characterizations. |
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