ZSM-5 molecular sieve containing phosphorus in crystal, synthetic method and application thereof
A ZSM-5, synthesis method technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problems of high price, affecting the catalytic activity of molecular sieve catalysts, and affecting the stability of molecular sieves. The effect of catalytic activity
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[0021] A method for synthesizing ZSM-5 molecular sieves containing phosphorus in crystals, comprising the following steps:
[0022] (1) Mix the quaternary ammonium base, tetrabutylphosphorus hydroxide and the aluminum source. The mixture is treated in a closed reaction kettle at 50-190°C for 0.1-5 hours and then cooled to obtain an intermediate product. The aluminum source does not contain alkali Aluminum source of metal ions;
[0023] (2) mixing the intermediate product of step (1) with silicon source and water to obtain a mixture;
[0024] (3) The mixture in step (2) is placed in a closed reactor for hydrothermal crystallization and the product is recovered.
[0025] In the synthetic method provided by the invention, in the mixture described in step (1), the sum of the moles of quaternary ammonium base and tetrabutylphosphorus hydroxide 2 o 3 The ratio of the number of moles of the aluminum source is 0.2 to 40:1; preferably, the sum of the number of moles of the quaternar...
Embodiment 1
[0050] This example illustrates the synthetic method provided by the present invention.
[0051] Weigh 0.21 gram of pseudo-boehmite (Hunan Jianchang Company, Al 2 o 3 content 70.11%), with 16.56g tetramethylammonium hydroxide aqueous solution (Beijing Jiayousheng New Technology Development Center, analytically pure, TMAOH content 10%) and 4.08g tetrabutylphosphine hydroxide (TBPOH, Sinopharm Chemical Reagent Co., Ltd. company, content 40%,) mixing, mixture molar ratio TMAOH / TBPOH=3, organic template agent / Al 2 o 3 = 10.6.
[0052] It was placed in a crystallization kettle containing a polytetrafluoroethylene liner, cooled to room temperature after reacting for 3 hours at 150° C., and then mixed with 30 g of silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99% solid content 92%) mixes with 33.20g water, mixture molar ratio SiO 2 / Al 2 o 3 =200,H 2 O / SiO 2 = 6.5. The mixture was subjected to hydrothermal crystallization at 120° C. for 73 hours in an autoclav...
Embodiment 2
[0062] This example illustrates the synthetic method provided by the present invention.
[0063] Weigh 0.5 gram of pseudo-boehmite (Hunan Jianchang Company, Al 2 o 3content 75%), it was mixed with 8.36g tetraethylammonium hydroxide aqueous solution (Shanghai Yongsheng Reagent Factory, analytically pure, TEAOH content 40%) and 4.71g tetrabutylphosphine hydroxide (TBPOH, Sinopharm Group Chemical Reagent Co., Ltd., content 40%) %) mixed, mixture molar ratio TEAOH / TBPOH=3.33, organic template / Al 2 o 3 = 6.5. It was placed in a crystallization kettle containing a polytetrafluoroethylene lining, cooled to room temperature after reacting for 2 hours at 150°C, after that, it was mixed with 30g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99% solid content 92%) mixes with 54.9g water, mixture molar ratio SiO 2 / Al 2 o 3 =100,H 2 O / SiO 2 =8. The mixture was subjected to hydrothermal crystallization at 130° C. for 40 hours in an autoclave. After crystallization,...
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