Method for aluminum incorporation into high-silica zeolites prepared in fluoride media
A technology of silica and zeolite, applied in the field of alumina source, can solve problems such as limitation
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Embodiment 1
[0134] Example 1. Synthesis of organic SDA for the production of LTA-type zeolites.
[0135] 4-Methyl-2,3,6,7-tetrahydro-1H,5H-pyrido[3.2.1-ij]quinolinium hydroxide (methylated julolidine) was used as the seed for the synthesis and SDA of high silica LTA type zeolites. Synthetic procedures were as described previously. Typically, 10 g of julonidine is dissolved in 100 ml of chloroform. 23 g of iodomethane was added to the solution, and the reaction mixture was stirred at room temperature for 3 days. Then, another 23 g of iodomethane were added to the solution, and the solution was stirred at room temperature for another 3 days. The same procedure was repeated again (addition of the same amount of iodomethane and stirring at room temperature for 3 days), the total reaction time was 9 days. A solid was obtained by slowly adding diethyl ether (-200ml) to the solution. The dark orange solid precipitated was filtered and air dried. The solid product was purified by redissolvi...
Embodiment 2
[0136] Example 2. Synthesis of organic SDA for ITW type zeolites.
[0137] 1,2,3-Trimethylimidazolium hydroxide was used as the synthetic seed and organic SDA of high-silica ITW-type zeolites. Synthetic procedures were as described previously. Typically, 8 g of 1,2-dimethylimidazole is dissolved in 100 ml of chloroform. 30 g of iodomethane was added to the solution, and the reaction mixture was stirred at room temperature for 2 days. The white-orange solid precipitated was filtered, washed with chloroform, and dried at room temperature. Organic SDA in the iodide form was ion-exchanged to the hydroxide form using ion-exchange resins prior to use in zeolite synthesis. About 5 g of resin was used in 50 g of SDA iodide solution (0.2M). The ion exchange step was performed at room temperature for 1 day, and this step was repeated three times. This yielded about 70% conversion of the iodide form to the hydroxide form. It is not possible to increase the ion exchange level above ...
Embodiment 3
[0138] Example 3. Synthesis of quasi-silicon LTA-type seed crystals.
[0139]The quasi-silicon seeds were synthesized by adding a total amount of about 5 wt% of silica formed from TEOS of germanosilicate ITQ-29 crystals to the reaction mixture in the synthesis procedure for pure silica ITQ-29 (Si / Ge=120). Germanosilicate ITQ-29 was synthesized by hydrothermal reaction of condensed reactive gels, as described in previous reports. The XRD pattern of the fabricated Ge-ITQ-29 is shown in figure 2 middle. In the synthesis of quasi-siliceous seeds, in a solution containing a mixture of methylated julonidine hydroxide (ROH) and tetramethylammonium hydroxide (TMAOH, 25% in water, Alfa Aesar), under stirring Tetraethylorthosilicate (TEOS) was hydrolyzed at room temperature for 3 hours. After the solution became homogeneous, the prepared germanosilicate ITQ-29 (5 wt% of the total silica formed from TEOS) was added to the solution and stirred for 1 h. Hydrofluoric acid (HF, 48-51% ...
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