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A kind of preparation method of phosphorus-containing multi-stage porous zsm-5/y composite molecular sieve

A composite molecular sieve, ZSM-5 technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of low yield of low-carbon olefins, low catalyst cracking activity, etc., to achieve high selectivity, good Industrial application prospects and economic value, the effect of low raw material cost

Active Publication Date: 2021-01-22
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 preparation method of phosphorus-containing hierarchically porous ZSM-5 / Y composite molecular sieve, which is simple to operate, low in raw material cost, and effectively solves the problem of low catalyst cracking activity and low carbon in existing FCC units. To solve the technical problem of low olefin yield, effectively obtain high-selectivity propylene, and improve the product composition of the catalytic cracking process unit

Method used

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  • A kind of preparation method of phosphorus-containing multi-stage porous zsm-5/y composite molecular sieve
  • A kind of preparation method of phosphorus-containing multi-stage porous zsm-5/y composite molecular sieve

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Embodiment 1

[0050] The embodiment of the present invention provides a preparation method of a phosphorus-containing hierarchical porous ZSM-5 / Y composite molecular sieve, comprising the following steps:

[0051] (1) 236.6g H 2 O, 9.1g NaOH, 138.7g TPAOH are mixed to form a solution, add 5.0g NaY molecular sieve (silicon-aluminum ratio is 5.3) and mix well, then add 372.3g silica sol and 1.24g boric acid to the above solution gradually in batches under full stirring And shake vigorously at room temperature for 1 hour, the molar ratio in the mixed slurry is:

[0052] 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

[0053] Then put the material in a PTFE-lined stainless steel reaction kettle, crystallize at 180°C for 24 hours, filter and wash the product until the pH value is 7-8, dry at 120°C for 12 hours, and roast at 550°C for 2 hours to obtain NaZSM-5 / Y compound molecular sieve.

[0054] (2) use the NaZSM-5 / Y molecular sieve that 10g step (1) obtains ...

Embodiment 2-8

[0057] Embodiments 2-8 of the present invention respectively provide a preparation method of phosphorus-containing hierarchically porous ZSM-5 / Y composite molecular sieves. The types of silicon source, boron source, organic template agent, phosphorus source and ammonium salt selected are as follows: As shown in Table 1, conventional industrial NaY molecular sieves (silicon-aluminum ratio of 5.3) are used to provide aluminum source and additional silicon source, and the same process method as in Example 1 is used for preparation. The composition of the compound molecular sieve crystallization precursor mixture obtained is shown in Table 1 shown. The finally prepared samples are designated as PZ5Y-2 to PZ5Y-8.

[0058] Table 1

[0059]

[0060] The physical and chemical characterization parameters of the sample PZ5Y-1-8 prepared in Example 1-8 and the sample VS-1-3 prepared in Comparative Example 1-3 are shown in Table 2.

[0061] Table 2

[0062]

Embodiment 9-19

[0064]Examples 9-16 of the present invention respectively provide a method for using samples PZ5Y-1-PZ5Y-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 of using the samples VS-1~VS-3 prepared in Comparative Examples 1-3 as a catalyst to catalytically crack naphtha to produce ethylene and propylene is provided, and the catalyst samples PZ5Y-1~PZ5Y-8 are tested by this method Evaluation was performed with VS-1 to VS-3.

[0065] 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, the inner diameter is 19 mm, and a thermocouple sleeve with an outer diameter of 6 mm is built in. The loading amount of the catalyst is 10g, and the particle size is 20-40 mesh. Naphtha and water...

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Abstract

The invention discloses a preparation method of a phosphorus-containing multi-level porous ZSM-5 / Y composite molecular sieve, which comprises the following steps: mixing an alkali, an organic template agent and deionized water into a solution, adding NaY molecular sieve, adding a silicon source and Boron source, obtain mixed sol crystallization, remove the template agent after recovering the crystallization product, obtain NaZSM‑5 / Y composite molecular sieve; then carry out ammonium ion exchange in ammonium salt solution to remove Na ion, obtain NH4‑ZSM‑5 / Y Y composite molecular sieve; then remove the boron element in the skeleton, and impregnate with phosphide to obtain phosphorus-containing ZSM‑5 / Y composite molecular sieve. The beneficial effects of the present invention are: the preparation method is simple to operate, low in cost and environmentally friendly; the composite molecular sieve of the present invention has micropores and mesoporous structures while having different silicon-aluminum ratios; using the composite molecular sieve of the present invention as a catalyst can solve the problem of existing catalytic In the cracking (FCC) unit, there are technical problems of low catalyst cracking activity and low yield of low-carbon olefins, so as to effectively obtain high-selectivity propylene and improve the product composition of the catalytic cracking process unit.

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-containing multi-stage porous ZSM-5 / Y composite molecular sieves. Background technique [0002] At present, the production of light olefins from petroleum as raw materials is mainly produced through hydrocarbon steam cracking and catalytic cracking processes. Traditional steam cracking is carried out by free radical reaction, with high temperature and strict requirements on raw materials. The cost of producing low-carbon olefins by catalytic cracking is relatively low, and it plays an increasingly important role in the production of propylene. In the catalytic cracking process, catalysts are used to catalytically crack heavy hydrocarbon fractions, such as vacuum gas oil (VGO), and the hydrocarbons are cracked to generate gasoline, light olefins, LPG and dry gas. Light olefins, especially propylene, are increasing...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/80C01B39/40C01B39/24C10G70/00
CPCC10G70/00C01B39/24C01B39/40B01J29/084B01J29/40B01J29/80B01J2229/186B01J2229/62C10G2400/20Y02P20/52
Inventor 于心玉王志光石文记魏胜华
Owner SHANDONG DUOYOU TECH
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