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Preparation method of phosphorus-containing multilevel 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 equipment requirements

Active Publication Date: 2018-11-06
SHANDONG DUOYOU TECH
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  • 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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  • Preparation method of phosphorus-containing multilevel porous ZSM-5/Y composite molecular sieve
  • Preparation method of phosphorus-containing multilevel porous ZSM-5/Y composite molecular sieve

Examples

Experimental program
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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 multilevel porous ZSM-5 / Y composite molecular sieve. The preparation method comprises the following steps: mixing alkali, an organic template and deionized water to form a solution; adding a NaY molecular sieve and adding a silicon source and a boron source to obtain a mixed sol, crystallizing, recovering a crystallized product and then removing the template to obtain a NaZSM-5 / Y composite molecular sieve; then performing ammonium exchange in an ammonium salt solution to remove a Na ion to obtain a NH4-ZSM-5 / Y composite molecular sieve; and removing a boron element in a skeleton, and impregnating with a phosphide to obtain the phosphorus-containing multilevel porous ZSM-5 / Y composite molecular sieve. The preparation method has the beneficial effects that the preparation method is simple to operate, low in cost and environmentally friendly; the composite molecular sieve has different silica-alumina ratios and is ofa microporous and mesoporous structure; the composite molecular sieve is used as a catalyst, so that the technical problems that an existing fluid catalyst cracking (FCC) unit has the disadvantages that the catalyst cracking activity is low and the low-carbon olefin yield is low can be solved, high-selectivity propylene is effectively obtained, and the product composition of the catalytic crackingtechnical unit is improved.

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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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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