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Al–Si-beta and Ti–Si-beta were synthesized by the aging–drying method in fluoride medium without seeding and using tetraethylammonium hydroxide as organic structure-directing agent (OSDA). In the aging–drying method the gels are allowed to release some volatile species (mainly ethanol and water).Samples were aged and dried during about one week. Organic solvents were added to selected aged–dried gels to determine their role as complementary OSDA. All samples were hydrothermally treated at 140 ℃ during 1–12 days. After crystallization, samples were characterized by PXRD, SEM, TGADTG, FTIR, atomic absorption, low temperature nitrogen adsorption, 29Si MAS NMR and 27Al MAS NMR. Pure and well-crystallized zeolite beta samples were obtained in all experiments performed. Polymorph A enrichments of about 69% and 64% were reached for Ti and Al loaded samples, respectively. Al-loaded samples exhibited small average crystal sizes compared with Ti-loaded samples. The incorporation of Al in the beta framework was proven by several techniques and the Al/Si ratios were similar to those of the precursor gels. However, Ti incorporation was quite low. |
| Al–Si-β和Ti–Si-β在氟化物介質中在不接種和使用氫氧化四乙銨作為有機結構導向劑(OSDA)情況下,通過老化-干燥法合成。在老化-干燥法中,允許硅膠釋放一些揮發(fā)物種(主要是乙醇和水)。在約一周時間里,樣本被老化和干燥。有機溶劑被加入選定的老化-干燥的硅膠中,以測定他們作為輔助OSDA的作用。所有的樣本在1-12天的時間在140C進行熱液處理。結晶后,通過PXRD、SEM、TGADTG、FTIR、原子吸收、低溫氮吸收、29Si MAS NMR和27Al MAS NMR去定它的具體特征。在進行所有的實驗中,獲得存的和良好結晶的沸石β樣本。Ti和Al實驗的樣本分別達到約69%和64%的多形體A富集。Al實驗樣本較Ti實驗樣本現實較小的結晶尺寸。在β框架中引入Al已經被若干技術證明,并且Al/Si的比例與前體硅膠相似。然而,引入Ti是相當的低。 |
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