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MFI structure molecular sieve containing phosphorus and transition metals, 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

Active Publication Date: 2012-12-26
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] However, the existing MFI structural molecular sieves modified by phosphorus and transition metals are used as catalysts or active components of catalysts for catalytic cracking of hydrocarbon oils. Although they can increase the yield and selectivity of propylene, the yields of dry gas and coke are relatively high.

Method used

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  • MFI structure molecular sieve containing phosphorus and transition metals, and preparation method thereof
  • MFI structure molecular sieve containing phosphorus and transition metals, and preparation method thereof
  • MFI structure molecular sieve containing phosphorus and transition metals, and preparation method thereof

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preparation example Construction

[0033] The calcined MFI structure molecular sieve containing phosphorus and transition metal can be prepared by introducing phosphorus and transition metal into MFI structure molecular sieve (eg, ammonium type or hydrogen type MFI structure molecular sieve) and calcining. The introduction of phosphorus and transition gold can impregnate the MFI molecular sieve with a solution containing phosphorus and transition metal. The solution of the phosphorus compound is impregnated, and the impregnation can be carried out one or more times, ie, the phosphorus and the transition metal can be introduced one or more times. The way of impregnation can be saturated impregnation or supersaturated impregnation. A preferred preparation method may include: mixing and impregnating ammonium type and / or hydrogen type MFI molecular sieve with calculated amounts of phosphorus-containing compound solution and transition metal-containing compound solution at room temperature (usually 15-30° C.) to 95°...

specific Embodiment approach

[0035] A specific embodiment of the preparation method provided by the present invention includes:

[0036] (1) According to molecular sieve: ammonium salt: H 2 The weight ratio of O=1:(0.1~1):(5~10): The sodium type MFI molecular sieve is exchanged at room temperature to 100°C for 0.3~1 hour, then filtered and dried;

[0037] (2) Impregnate the ammonium-exchanged molecular sieve with a solution containing a phosphorus-containing compound and a solution containing a transition metal compound, then dry and roast it; the roasting temperature is 400-800°C; the phosphorus-containing compound solution and the transition metal The impregnation of the ammonium-exchanged molecular sieve with the metal compound solution can be impregnated with a solution containing both a phosphorus compound and a transition metal compound, or impregnated with a solution containing a phosphorus compound and a solution containing a transition metal compound respectively; Can be done one or more times. ...

Embodiment 1

[0041] 50g NH 4 Cl was dissolved in 1000g of water, and 100g (dry basis) of the crystallized product ZSM-5 molecular sieve (produced by Sinopec Catalyst Qilu Branch, synthesized by amine method, SiO 2 / Al 2 O 3 =50), after 0.5h exchange at 90°C, filter cake; 9.0g H 3 PO 4 (concentration 85 wt%) with 8.1 g Fe (NO 3 ) 3 ·9H 2 O is dissolved in 90g water, this dipping solution is mixed with filter cake and dipped, oven-dried, and calcined at 550 ° C for 2 hours; get 10g of the above calcined molecular sieve, mix it with 5.36g of ethyl orthosilicate (Beijing Chemical Reagent Company, Analytical pure, SiO 2 content 28% by weight), 3.33g of tetrapropylammonium bromide (produced by Guangzhou Dayou Fine Chemical Factory, analytically pure, 99% by weight) and 12ml of water were mixed, placed in a crystallization kettle containing polytetrafluoro lining, After static crystallization at 150° C. for 20 hours, it was cooled to room temperature, and then, the molecular sieve was dri...

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Abstract

The invention relates to a MFI structure molecular sieve containing phosphorus and transition metals, and a preparation method thereof. According to the MFI structure molecular sieve of the present invention, phosphorus distribution D meets the following conditions that D is more than or equal to 0 and less than or equal to 0.8, and is equal to P(S) / P(C), wherein P(S) represents the phosphorus content in a part from the edge to 1 / 5 of the center of the molecular sieve grain characterized by using a TEM-EDX method, P(C) represents the phosphorus content in the center of the molecular sieve grain, and no absorption peak exists at 1633 cm<-1> on an infrared spectrogram obtained by adopting 3-methylpyridine as a probe. The preparation method for the molecular sieve comprises: mixing the calcined MFI structure molecular sieve containing phosphorus and transition metals with a silicon source, carrying out reaction crystallization for 2-80 hours at a temperature of 145-190 DEG C, carrying out separating and drying, and carrying out calcination at a temperature of 400-800 DEG C. The molecular sieve of the present invention is used for catalytic cracking, wherein light olefin yield is high, and yields of coke, hydrogen and dry gas are reduced.

Description

technical field [0001] The invention relates to an MFI structure molecular sieve containing phosphorus and transition metals and a preparation method thereof. Background technique [0002] The typical representative of molecular sieves with MFI structure is the ZSM-5 zeolite developed by Mobil Corporation in the United States in the early 1970s. It has a unique pore structure and is widely used in alkylation, isomerization, disproportionation, catalytic cracking, and catalytic dewaxing. Wait for the reaction process. Catalytic cracking is one of the important production processes for producing light olefins. For most catalytic cracking units, in order to increase the production of propylene and butene, it is an effective method to use catalysts or additives containing molecular sieves with MFI structure. [0003] USP 3,758,403 discloses the addition of ZSM-5 molecular sieves as an active component in catalytic cracking catalysts. This method can increase the octane number ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85
Inventor 秦金来欧阳颖罗一斌舒兴田李明罡
Owner CHINA PETROLEUM & CHEM CORP
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