L-type molecular sieve containing germanium and preparation method thereof
A molecular sieve, L-type technology, applied to germanium-containing molecular sieves and the fields of preparation and application, can solve problems such as no relevant reports on the aromatization performance of alkanes, and achieve the effect of good aromatization activity
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preparation example Construction
[0020] The preparation method of the L-type molecular sieve provided by the invention comprises:
[0021] Mix the inorganic base, germanium source, aluminum source, silicon source and water to obtain a reaction gel; wherein, the molar composition of the reaction gel is: (6-20) SiO 2 :Al 2 o 3 : (0.01-0.12)GeO 2 :(1-6)M:(80-300)H 2 O;
[0022] The obtained reaction gel is subjected to hydrothermal crystallization, and the solid product obtained after crystallization is washed and dried.
[0023] Preferably, the molar composition of the reaction gel is: (10-15) SiO 2 :Al 2 o 3 : (0.04-0.10)GeO 2 :(2-6)M:(140-300)H 2 O.
[0024] In the method of the present invention, H 2 The molar ratio of O to M is preferably not more than 75.
[0025] In the method of the present invention, the temperature of the hydrothermal crystallization can be 100-200°C, preferably 150-180°C, the time is 10-200 hours, preferably 24-72 hours, and the drying temperature can be 80-120°C , the ti...
example 1
[0039] Example 1 Preparation of the directing agent used in the present invention.
[0040] Example 1
[0041] Preparation of directing agent
[0042] According to the molar composition of the feeding mixture, it is 8K 2 O·Al 2 o 3 14SiO2 2 ·320H 2 For the formula of O, 6g of hydrated alumina (the content of alumina is 70% by mass, the same below) was added to 132g of the solution containing 36.89g of KOH, heated and dissolved to obtain a mixed solution. With stirring, the mixed solution was added to 138 g of silica sol (containing 25% by mass SiO) preheated to 50° C. 2 , the pH value is 9, the same below), stirred for 0.5 hours to form a reaction gel, and aged the reaction gel at 34°C for 72 hours to obtain a translucent sol, which was used as a directing agent.
example 2
[0048] The germanium-containing L-type molecular sieve of the present invention is prepared.
[0049] Add 5.01g of hydrated alumina to 43.50g containing 9.97gKOH and 0.19gGeO 2 In the solution, heated and dissolved to obtain a mixed solution, the mixed solution was added to 81.52g of silica sol under stirring, and 8.08g of the directing agent prepared in Example 1 was added, and stirred for 0.5 hours to form a reaction gel, and its molar composition was: 10SiO 2 ·Al 2 o 3 0.05GeO 2 2.75K 2 O·160H 2 O, Al in the directing agent 2 o 3 Al in the reaction gel 2 o 3 The molar ratio is 3.0%.
[0050] Transfer the above reaction gel into the reaction kettle and crystallize at 170°C for 72 hours, then rapidly cool to 40°C, the product is centrifuged and washed until the pH value of the liquid phase is 10-11, and the obtained solid is dried at 120°C for 10 hours to obtain Germanium-containing L-type molecular sieve raw powder GL-1, its X-ray powder diffraction analysis spectr...
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