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Phosphorus-containing MFI structure molecular sieve and preparation method thereof

A molecular sieve and nanotechnology, applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of adding template agent, high cost, complexity and other problems, reduce coking deactivation, improve cracking activity, Mesoporous rich effect

Active Publication Date: 2018-05-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method needs to add a template agent and the process is complicated and the cost is high

Method used

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preparation example Construction

[0031] The present invention also provides a preparation method of the phosphorus-containing MFI structure molecular sieve provided by the present invention, the preparation method comprising: a, sodium type MFI structure molecular sieve is desiliconized in an alkaline solution to obtain a desiliconization molecular sieve; b, the step The desiliconized molecular sieve obtained in a is subjected to ammonium exchange to obtain an ammonium exchanged molecular sieve; wherein, in terms of sodium oxide and based on the total dry weight of the ammonium exchanged molecular sieve, the sodium content of the ammonium exchanged molecular sieve is less than 0.2% by weight; c. The ammonium-exchanged molecular sieve obtained in step b is dealuminated in a complex acid dealumination agent solution composed of fluosilicic acid, organic acid and inorganic acid, and after filtering and washing, the dealuminated molecular sieve is obtained; d. After the obtained dealuminated molecular sieve is sub...

Embodiment 1

[0059] Crystallized ZSM-5 molecular sieve (produced by Catalyst Qilu Branch Company, synthesized without amine method, n(SiO 2 ) / n(Al 2 o 3 )=27) filter out mother liquor, wash with water to Na 2 O content is lower than 3.0% by weight, filter to obtain filter cake; Take above-mentioned molecular sieve 100g (dry basis) and add in 1000g 2.0% NaOH solution, heat up to 65 ℃, after reacting for 30min, after rapidly cooling to room temperature, filter, wash to filtrate neutral. Then, add 800g water to the filter cake to make a slurry, add 40g NH 4 Cl, heated to 75°C, exchanged for 1h, to Na 2 O content is lower than 0.2% by weight, filters, washes, obtains molecular sieve filter cake; Get above-mentioned molecular sieve 50g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add oxalic acid 4g in stirring, then 45g hydrochloric acid (mass fraction 10%) and 30g of fluosilicic acid (mass fraction 3%) were added in parallel, and t...

Embodiment 2

[0079] Crystallized ZSM-5 molecular sieve (produced by Catalyst Qilu Branch Company, synthesized without amine method, n(SiO 2 ) / n(Al 2 o 3 )=27) filter out mother liquor, wash with water to Na 2 O content is lower than 3.0% by weight, filter to obtain filter cake; Get above-mentioned molecular sieve 100g (dry basis) and add in 1500g 2.3% NaOH solution, heat up to 60 ℃, after reacting for 45min, after rapidly cooling to room temperature, filter, wash to filtrate neutral. Then, add 800g water to the filter cake to make a slurry, add 40g NH 4 Cl, heated to 75°C, exchanged for 1h, to Na 2 O content is lower than 0.2% by weight, filters, washes, obtains molecular sieve filter cake; Get above-mentioned molecular sieve 50g (dry basis) and add water and be mixed with the molecular sieve slurry of solid content 10% by weight, add citric acid 4g in stirring, then 10g sulfuric acid (mass fraction 10%) and 45g of fluosilicic acid (mass fraction 3%) were added in parallel, and the ad...

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Abstract

The invention discloses a phosphorus-containing MFI structure molecular sieve and a preparation method thereof, wherein the n(SiO2) / n(Al2O3) of the molecular sieve is more than 18 and is less than 70,the phosphorus content (calculated as P2O5) of the molecular sieve is 1-15 wt% by using the dry base weight of the molecular sieve as the reference, the volume of the mesopores of the molecular sieveaccounts for 40-70% of the total pore volume, the volume of the mesopores with the pore size of 2-20 nm accounts for more than 85% of the total mesopore volume, the amount of the strong acid of the molecular sieve accounts for 45-75% of the total acid amount, and a ratio of the acid B to the acid L is 8-30. According to the present invention, with the catalyst or the auxiliary agent prepared by using the phosphorus-containing MFI structure molecular sieve as the active component, the propylene yield and the propylene selectivity can be effectively increased in the catalytic cracking or catalytic cracking reaction of petroleum hydrocarbons while the yield of BTX can be increased.

Description

technical field [0001] The invention relates to a phosphorus-containing MFI structure molecular sieve and a preparation method thereof. Background technique [0002] For a long time, ethylene, propylene and butene have been the basic organic chemical raw materials for synthetic resin, synthetic fiber and synthetic rubber, among which propylene is an important raw material for the manufacture of petrochemical products after ethylene. At present, the largest source of propylene at home and abroad is the main by-product of thermal cracking to produce ethylene. Liquid-based ethylene plants usually produce about 15% of propylene, providing about 70% of the propylene consumed by the petrochemical industry, while the second largest source of propylene is almost all from FCC units, providing about 30% of demand, In the United States, FCC units provide about half of petrochemicals' propylene demand. [0003] Due to the rapidly growing demand for polypropylene, the demand for propyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/40
CPCB01J29/40C01B39/026C01B39/38C01P2006/14C01P2006/16C01P2006/17
Inventor 庄立欧阳颖罗一斌刘建强舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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