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Method for preparing phosphorus modified ZSM-5 molecular sieve with hierarchical pores

A ZSM-5, molecular sieve technology, applied in molecular sieve catalysts, including molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of low yield of low-carbon olefins, low catalyst cracking activity, etc., and achieve high selectivity and good industrial application. Prospects and economic value, the effect of low cost of raw materials

Active Publication Date: 2018-11-02
SHANDONG DUOYOU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a phosphorus-modified ZSM-5 molecular sieve with hierarchical pores and a preparation method thereof. The preparation method is simple in operation and low in raw material cost, and can effectively solve the problem of low catalyst cracking activity and low-carbon olefins in existing FCC units. The technical problem of low yield, effectively obtain highly selective propylene, and improve the product composition of the catalytic cracking process unit

Method used

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  • Method for preparing phosphorus modified ZSM-5 molecular sieve with hierarchical pores
  • Method for preparing phosphorus modified ZSM-5 molecular sieve with hierarchical pores
  • Method for preparing phosphorus modified ZSM-5 molecular sieve with hierarchical pores

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Embodiment 1

[0038] The embodiment of the present invention provides a method for preparing a phosphorus-modified ZSM-5 molecular sieve with hierarchical pores, comprising the following steps:

[0039] (1) 281.6g H 2 O, 11.9g NaOH, 169.5g TPAOH (concentration 25wt%) and 1.57g pseudo-boehmite (Al 2 o 3 %: 65wt%) were mixed into a solution, and then 466.4g of silica sol and 1.24g of boric acid were gradually added to the above solution in batches under full stirring and vigorously shaken at room temperature for 1 hour to obtain the molar ratio in the mixed sol:

[0040] Na 2 O:SiO 2 :Al 2 o 3 :B 2 o 3 :OSDA:H 2 O=0.075:1:0.0048:0.0198:0.1:20

[0041] Then the obtained mixed sol was placed in a PTFE-lined stainless steel reaction kettle, crystallized at 160°C for 72 hours, the product was filtered and washed until the pH value was 7-8, dried at 120°C for 12 hours, and calcined at 550°C for 2 hours to obtain NaZSM-5 molecular sieve.

[0042] (2) Use 10g of the NaZSM-5 molecular siev...

Embodiment 2-8

[0045] Embodiments 2-8 of the present invention respectively provide a preparation method of a phosphorus-modified ZSM-5 molecular sieve with hierarchical pores, the selected silicon source, aluminum source, boron source, organic template agent, phosphorus source and ammonium salt The types are shown in Table 1, prepared by the same process as in Example 1, the composition of the obtained synthetic molecular sieve crystallization precursor mixture is shown in Table 1 and Table 2, and the physicochemical characterization parameters of the obtained product are shown in Table 2.

[0046] Table 1

[0047]

[0048]

[0049] Table 2

[0050]

Embodiment 9-19

[0052] Examples 9-16 of the present invention respectively provide a method for using samples PZ5-1 to PZ5-8 prepared in Examples 1-8 as catalysts to catalytically crack naphtha to produce ethylene and propylene. Examples 17-19 of the present invention A method for using the samples VS-1~VS-3 prepared in Comparative Examples 1-3 as a catalyst to catalyze the cracking of naphtha to produce ethylene and propylene is provided, and the catalyst samples PZ5-1~PZ5-8 are tested by this method Evaluation was performed with VS-1 to VS-3.

[0053] The catalyst was evaluated in a continuous flow fixed-bed reactor. The composition of the naphtha raw material is shown in Table 3, and the evaluation conditions and reaction results can be seen in Table 4. The material of the reactor is stainless steel, with an inner diameter of 19 mm and a built-in thermocouple sleeve with an outer diameter of 6 mm. The loading amount of the catalyst is 10g, and the particle size is 20-40 mesh. Naphtha and...

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Abstract

The invention discloses a method for preparing a phosphorus modified ZSM-5 molecular sieve with hierarchical pores. The method includes steps: well mixing an aluminum source, alkali, an organic template agent and deionized water, adding a silicon source and a boron source, crystallizing obtained mixed sol, recovering a crystallized product, an removing the template agent to obtain a NaZSM-5 molecular sieve; performing ammonium ion exchange to remove Na ions, subjecting obtained NH4-ZSM-5 molecular sieve to steam treatment to obtain a boron removed molecular sieve; impregnating in phosphorus compound solution, drying and calcining to obtain the phosphorus modified ZSM-5 molecular sieve with the hierarchical pores. The method has advantages that the ZSM-5 molecular sieve prepared according to the method serves as a cracking catalyst auxiliary agent to solve problems of low catalyst cracking activity and low carbon olefin yield in an existing catalytic cracking FCC unit, high-selectivitypropylene is obtained, and product composition is improved; in addition, the method is simple in operating step, low in equipment requirement, low in cost, environmentally friendly and promising in application prospect.

Description

technical field [0001] The invention relates to the field of molecular sieve materials and preparation thereof, in particular to a method for preparing phosphorus-modified ZSM-5 molecular sieves with hierarchical pores. Background technique [0002] ZSM-5 molecular sieve is a widely used zeolite molecular sieve catalytic material developed by Mobil Corporation of the United States in 1972. ZSM-5 molecular sieve has a three-dimensional intersecting channel structure. The channel along the a-axis is a straight hole with a cross-sectional size of 0.54×0.56nm, which is approximately circular. The channel along the b-axis is a zigzag hole with a cross-sectional size of 0.51 ×0.56nm, oval shape. Its orifice is composed of ten-membered rings, and its size is between small-pore zeolite and large-pore zeolite, so this type of molecular sieve has a unique shape-selective catalytic effect. It has a unique pore structure, good shape-selective catalysis and isomerization performance, h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B01J29/40C07C4/06C07C11/04C07C11/06
CPCB01J29/40B01J2229/18C01B39/40C01P2006/17C07C4/06C07C2529/40C07C11/04C07C11/06Y02P20/52
Inventor 于心玉王志光石文记魏胜华
Owner SHANDONG DUOYOU TECH
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