A kind of MFI structure molecular sieve containing phosphorus and loaded metal and preparation method thereof
A technology of loading metals and molecular sieves, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, molecular sieves and alkali exchange compounds, etc., can solve the problems of complexity, high cost, and template addition process, so as to strengthen the dehydrogenation function and increase the yield , Reduce the effect of coking and deactivation
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[0034] The present invention also provides a method for preparing the phosphorus-containing and metal-loaded MFI molecular sieve provided by the present invention, the preparation method comprising: a. The sodium-type MFI molecular sieve is desiliconized in an alkaline solution to obtain a desiliconized molecular sieve ; b, performing ammonium exchange on the desiliconized molecular sieve obtained in step a to obtain an ammonium exchanged molecular sieve; wherein, the sodium content of the ammonium exchanged molecular sieve is less than 0.2 wt. %; c, the ammonium-exchanged molecular sieve obtained in step b is dealuminated in a complex acid dealumination agent solution composed of fluosilicic acid, organic acid and inorganic acid, and after filtering and washing, the dealuminated molecular sieve is obtained; d . After the dealuminated molecular sieve obtained in step c is subjected to phosphorus modification treatment, metal-loaded modification treatment and roasting treatment,...
Embodiment 1
[0064] Crystallized ZSM-5 molecular sieve (produced by Catalyst Qilu Branch Company, synthesized without amine method, n(SiO 2 ) / n(Al 2 o 3 )=27) filter out mother liquor, wash with water to Na 2 O content is lower than 3.0% by weight, filter to obtain filter cake; Take above-mentioned molecular sieve 100g (dry basis) and add in 1000g 2.0% NaOH solution, heat up to 65 ℃, after reacting for 30min, after rapidly cooling to room temperature, filter, wash to filtrate neutral. Then, add 800g water to the filter cake to make a slurry, add 40g NH 4 Cl, heated to 75°C, exchanged for 1h, to Na 2 O content is lower than 0.2% by weight, filters, washes, obtains molecular sieve filter cake; Get above-mentioned molecular sieve 50g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add oxalic acid 4g in stirring, then 45g hydrochloric acid (mass fraction 10%) and 30g of fluosilicic acid (mass fraction 3%) were added in parallel, and t...
Embodiment 2
[0084] Crystallized ZSM-5 molecular sieve (produced by Catalyst Qilu Branch Company, synthesized without amine method, n(SiO 2 ) / n(Al 2 o 3 )=27) filter out mother liquor, wash with water to Na 2 O content is lower than 3.0% by weight, filter to obtain filter cake; Get above-mentioned molecular sieve 100g (dry basis) and add in 1500g 2.3% NaOH solution, heat up to 60 ℃, after reacting for 45min, after rapidly cooling to room temperature, filter, wash to filtrate neutral. Then, add 800g water to the filter cake to make a slurry, add 40g NH 4 Cl, heated to 75°C, exchanged for 1h, to Na 2 O content is lower than 0.2% by weight, filters, washes, obtains molecular sieve filter cake; Get above-mentioned molecular sieve 50g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add citric acid 4g in stirring, then 10g sulfuric acid (mass fraction 10%) and 45g of fluosilicic acid (mass fraction 3%) were added in parallel, and the ad...
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