A kind of phosphorus-containing MFI structure molecular sieve and preparation method thereof
A molecular sieve and ammonium exchange technology, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor hydrothermal stability, difficult production, high discharge of three wastes, etc., and achieve weak cracking ability and keep gasoline Effect of octane number and improvement of gasoline yield
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[0038] The present invention also provides a preparation method of the phosphorus-containing MFI structure molecular sieve, the method comprising: a. performing ammonium exchange on the sodium type MFI structure molecular sieve to obtain ammonium exchange molecular sieve; The total dry basis weight is the basis, and the sodium content of the ammonium-exchanged molecular sieve is less than 0.2% by weight; b, the ammonium-exchanged molecular sieve obtained in step a is placed in a complex acid dealuminizing agent solution composed of fluosilicic acid, organic acid and inorganic acid After dealumination, filtration and washing, the dealumination molecular sieve is obtained; c, after the dealumination molecular sieve obtained in step b is subjected to phosphorus modification treatment and roasting treatment, the phosphorus-containing MFI structure molecular sieve is obtained.
[0039] According to the method of the present invention, the sodium-type MFI molecular sieve is well know...
Embodiment 1
[0061] With ZSM-5 molecular sieve (catalyst Qilu branch production, no amine synthesis, n(SiO 2 ) / n(Al 2 o 3 )=27) with NH 4 Cl solution exchange wash to Na 2 O content is lower than 0.2% by weight, filters to obtain filter cake; Get above-mentioned molecular sieve 100g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add oxalic acid 20g in stirring, then 200g hydrochloric acid (mass fraction 10%) and 167g of fluosilicic acid (mass fraction 3%) was added in parallel, and the addition time was 30 minutes; the temperature was raised to 65°C and stirred for 1 hour, filtered and washed until the filtrate was neutral; the filter cake was beaten with water to obtain a molecular sieve slurry with a solid content of 40% by weight, and added 2.4gH 3 PO 4 (Concentration: 85% by weight), homogeneously mixed and dipped, dried, and roasted at 550° C. for 2 hours. Molecular sieve A was obtained, and the physical and chemical proper...
Embodiment 2
[0077] With ZSM-5 molecular sieve (catalyst Qilu branch production, no amine synthesis, n(SiO 2 ) / n(Al 2 o 3 )=27) with NH 4 Cl solution exchange wash to Na 2 O content is lower than 0.2% by weight, filters to obtain filter cake; Get above-mentioned molecular sieve 100g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add citric acid 40g in stirring, then add 100g sulfuric acid (mass fraction 10%) and 500g of fluosilicic acid (3% by mass) were added in parallel, and the addition time was 30min; the temperature was raised to 45°C and stirred for 1h, filtered and washed until the filtrate was neutral; the filter cake was beaten with water to obtain a molecular sieve slurry with a solid content of 40% by weight, Add 2.0gH 3 PO 4 (Concentration: 85% by weight), homogeneously mixed and dipped, dried, and roasted at 550° C. for 2 hours. Molecular sieve B was obtained, and the physical and chemical properties, micro-reaction...
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