A kind of MFI structure molecular sieve containing phosphorus and transition metal and preparation method thereof
A technology of transition metals and molecular sieves, applied in the direction of molecular sieve catalysts, chemical instruments and methods, molecular sieves and alkali-exchanged phosphates, etc., can solve the problems of high yields of dry gas and coke, and achieve high and low carbon olefins yield and selectivity, high yield rate and the effect of selectivity
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[0033] The calcined MFI structure molecular sieve containing phosphorus and transition metals can be prepared by introducing phosphorus and transition metals into MFI structure molecular sieves (such as ammonium-type or hydrogen-type MFI structure molecular sieves) and calcining. The introduction of phosphorus and transition gold can impregnate MFI structure molecular sieves with a solution containing phosphorus and transition metals. The impregnation can be impregnated successively with a solution containing a transition metal compound and a solution containing a phosphorus compound, or can also be impregnated with a solution containing a transition metal compound and a solution containing a transition metal compound and The solution of the phosphorus compound is impregnated, and the impregnation can be carried out one or more times, that is, the phosphorus and the transition metal can be introduced once or several times. The way of impregnation can be saturated impregnation o...
specific Embodiment approach
[0035] A specific embodiment of the preparation method provided by the invention includes:
[0036] (1) According to molecular sieve: ammonium salt: H 2 O=1: (0.1~1): (5~10) weight ratio Sodium type MFI structure molecular sieve is exchanged at room temperature to 100 ℃ for 0.3~1 hour and then filtered and dried;
[0037] (2) Impregnating and modifying the ammonium-exchanged molecular sieve with a phosphorus-containing compound solution and a solution containing a transition metal compound, then drying and roasting; the roasting temperature is 400-800° C.; The metal compound solution impregnates the ammonium-exchanged molecular sieve, which may be impregnated with a solution containing both a phosphorus compound and a transition metal compound, or may be impregnated separately with a solution containing a phosphorus compound and a solution containing a transition metal compound; the impregnation Can be done one or more times. Preferably, the impregnation is performed with a ...
Embodiment 1
[0041] 50g NH 4 Cl was dissolved in 1000g water, and 100g (dry basis) crystallization product ZSM-5 molecular sieve (produced by Sinopec Catalyst Qilu Branch Company, produced by amine method, SiO 2 / Al 2 o 3 =50), after exchanging at 90°C for 0.5h, filtered to obtain a filter cake; 9.0g H 3 PO 4 (concentration 85% by weight) and 8.1g Fe(NO 3 ) 3 9H 2 O was dissolved in 90g of water, and the impregnating solution was mixed with the filter cake to impregnate, dried, and roasted at 550°C for 2 hours; take 10g of the above-mentioned roasted molecular sieve, and mix it with 5.36g of ethyl orthosilicate (Beijing Chemical Reagent Company, Analytical grade, SiO 2 content 28% by weight), 3.33g tetrapropylammonium bromide (Guangzhou Dayou fine chemical factory production, analytical pure, 99% by weight) and the mixture of 12ml water are mixed, are placed in the crystallization kettle that contains polytetrafluoroethylene liner, After static crystallization at 150°C for 20 hours...
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