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duyuhai铁杆木虫 (正式写手)
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[交流]
请问分子筛制备中水和Na2O的问题
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最近在试制Y型分子筛。 手册上讲到，feed gel的时候，给出了这样一个式子：10.67Na2O:Al2O3:10SiO2:180H2O 请问，这里的180H2O是经过计算得到的，还是后来测定的？制备这样的凝胶，所需的水的量真的只能按摩尔比算出是这样的么？ 另外，我按他投料比计算了一下Na2O的量不足这个比例。差不少。请问，NaOH的投料量是一定要按比例来还是可以多一些？？ 先谢谢了！ PS：如果哪位有Y型分子筛的详细制备步骤并且愿意共享，有更多金币相赠~ |
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dj_king
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FAU Linde Type Y Si(71), Al(29) Contributed by David Ginter Verified by G. Price andby C. Kuntz Type Material Na56[Al56Si136O384] : 250 H2O Method D. M. Ginter, A. T. Bell and C. J. Radke [1] Batch Compositiona Seed Gel (5% of Al): 10.67 Na2O : Al2O3 :10 SiO2 : 180 H2O Feed Stock Gel (95% of Al): 4.30 Na2O : Al2O3 : 10 SiO2:180 H2O Overall Gel: 4.62 Na2O : Al2O3 : 10 SiO2 : 180 H2O Source Materials deionized water sodium aluminate solid (Strem Chemicalb 1.27 Na/Al, 6.1% H2O) sodium hydroxide pellets (J. T.Baker, 99% NaOH) sodium silicate solution (PQ Corp, N Brand, 28.7 wt% SiO2, 8.9 wt% Na2O)c Batch Preparation (for 32 g anhydrous product) Seed Gel (1) [19.95 g water + 4.07 g sodium hydroxide + 2.09 g sodium aluminate], stir in 50 mL plastic bottle until dissolved (2) ((1) + 22.72 g sodium silicate solution], stir moderately for at least 10 minutes; after stirring, cap the bottle and let the solution age at room temperature for 1 dayd Feedstock Gele (3) [130.97 g water + 0.14 g sodium hydroxide + 13.09 g sodium aluminate], stir in a 500 mL plastic beaker until dissolved (4) [(3) 142.43 g sodium silicate solution], stir vigorously with a high-shear turbine mixerf until the gel appears somewhat smooth; cover the beaker until the addition of the seed gel Overall Gel (5) [(4) + 16.50 g of (2)], slowly add seed gel (2) to feedstock gel (4) under high shear;f move the beaker during mixing to ensure the entire gel volume encounters the high shear from the turbine (up to 20 minutes)g Crystallization Vessel: 300 mL polypropylene bottle (sealed) Incubation: One day at room temperature g Temperature: 1000C g Time: After about 5 h, the gel will separate into a solid (containing the NaY Zeolite) that will settle to the bottom, and a hazy supernatant liquid. Continue heating until the supernatant is clear indicating complete crystallization (no more than 2 additional hours)g Product Recovery (1) Centrifuge; decant supernatant (2) Filter the wet solid product; wash with distilled water until pH of filtrate is below 9 (3) Dry at ll0¡C (4) Yield: approximately 32 g of anhydrous NaY (about 98% on Al2O3) Product Characterization XRD FAU; characteristic strong reflections at d = 14.28, 8.75 and 7.46 Å, a0 = 24.72 Å. Competing phases (if present): GIS, GME, CHA Elemental Analysis; NaAlO2. 2.43 SiO2 Crystal Size and Habit: octahedral crystals, <1 um Click here to view XRD pattern References [1] D. M. Ginter, A. T. Bell, C. J. Radke, in Synthesis of Microporous Materials, Vol. 1, Molecular Sieves, M. L Occelli, H. E Robson (eds.), Van Nostrand Reinhold, New York, 1992, p 6 [2] T. Linder, C. Kurtz, personal communications Notes a. This procedure is reliable only for the production of submicron NaY crystals and is limited in the range of sizes and compositions that can be produced using slight procedural modifications. b. Also available as solutions with this Na/Al ratio from Alcoa and U. S. Aluminate. c. It should be clear of precipitated material. d. Solution is clear when prepared; during aging, a loose gel forms which contains the NaY seeds. e. May be prepared concurrently with the seed gel or just prior to mixing the overall gel. f. 1600 rpm with 2.5 inch diameter, 4 paddle radial mixer (minimum) recommended. g. If a GIS (NaP) impurity is produced, it can be eliminated by reducing the Na aluminate in (1) to 1.40 g and aging the seed gel for 1 to 5 days prior to blending it into the feedstock. Further aging of the composite is optional with this seed, and pure product has been obtained after crystallization at 900C for 22 hours [2] |
2楼2008-07-15 21:42:17
dj_king
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3楼2008-07-15 21:51:13
duyuhai
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buffaloli(金币+0,VIP+0):那上面的方太豪华了，呵呵
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不好意思，上面的确是我打错了。这个方法出自《Verified Synthesis of Zeolitic Materials》第二版。因为我的原料和他的不大一样，所以应该是要换算一下的。我按照它给出的方法计算出来的seed gel比例是：8.96Na2O : Al2O3 :10 SiO2 : 166 H2O（计算过程在后面，帮我看看有否漏掉什么，或者有计算错误。谢谢！），那么，究竟是按照他给出的原料折算，还是按照最后的胶体组成折算投料比呢？ 再一次感谢您！ ＰＳ，您把晶化温度贴错了，是１００℃，不是１０００Ｃ ---------------------------------------------------------------------------- 19.95 g H2O ~~~ H2O 1.10833 mol 4.07 g NaOH ~~ Na2O 0.050875 mol 2.09 g 偏铝酸钠中， 水有6.1%（应该是wt%）为 0.12749g 合 0.007083 mol Na/Al=1.27 ，应该符合(Na2O)1.27(AL2O3)（分子量：62*1.27+102=180.74），这部分质量为 2.09*0.939=1.96251 g 则，Na2O 1.96251/180.74*1.27= 0.013790 mol Al2O3 1.96251/180.74= 0.010858 mol 22.72 g 硅酸钠溶液中： SiO2：22.72*0.287=6.52064 g ~~ 0.108677 mol Na2O：22.72*0.089=2.02208g ~~ 0.032614 mol H2O ：22.72*0.624=14.17728g ~~ 0.787627 mol 这样 Na2O：0.050875(NaOH)+0.013790(偏铝酸钠)+0.032614(硅酸钠)=0.097279 mol Al2O3 ：0.010858 mol （只有偏铝酸钠的） SiO2 ：0.108677 mol （只有硅酸钠的） H2O ：1.10833(加的水)+0.007083(偏铝酸钠)+0.787627(硅酸钠溶液)=1.805573 mol 最后是8.96Na2O : Al2O3 :10 SiO2 : 166 H2O [ Last edited by duyuhai on 2008-7-16 at 19:33 ] |
4楼2008-07-16 17:00:37
dj_king
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5楼2008-07-16 22:14:18
6楼2008-07-17 16:40:32