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Process for producing cavity type ZSM-5 modified zeolite molecular sieve

A technology of modified zeolite and ZSM-5, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc. Structural diffusion channel narrow etc.

Active Publication Date: 2009-05-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is that there are narrow microporous structure diffusion channels in the prior art, the relative crystallinity of the modified zeolite molecular sieve is relatively low, and the adjustable range of the internal pores of the molecular sieve is small, which is not conducive to the reaction of macromolecules limited by diffusion. Provide a new cavity type ZSM-5 modified zeolite molecular sieve preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0015] Treat silicon aluminum molar ratio SiO with a concentration of 0.1, 1.0, 5.0 mol / liter hydrochloric acid or nitric acid solution at a temperature of 20, 50, and 90°C 2 / Al 2 o 3 110 ZSM-5 molecular sieve raw powder for 2, 5, and 8 hours, washed, dried, and then roasted at a temperature of 550°C; then at a temperature of 80°C, impregnated with a sodium carbonate solution with a concentration of 0.8 mol / liter for 24 hours, After washing and drying, roast at a temperature of 550°C; finally treat with a concentration of 0.1, 2.0, 5.0 mol / liter hydrochloric acid or nitric acid solution at a temperature of 40, 70, and 90°C for 2, 5, and 8 hours, wash, and dry The desired modified zeolite molecular sieve is obtained by calcining at a temperature of 550°C.

Embodiment 7～11

[0017] Treat the silicon-aluminum molar ratio SiO with a concentration of 1 mol / L hydrochloric acid solution at a temperature of 90°C 2 / Al 2 o 3 40, 110, 220, ZSM-5 molecular sieve raw powder with a particle size of 0.4, 2.0, and 8.0 microns for 5 hours, washed, dried, and roasted at a temperature of 550°C; then at a temperature of 20, 60, and 80°C, Sodium hydroxide, magnesium hydroxide, and sodium carbonate solutions with a concentration of 0.1, 0.6, 1.0, and 2.0 mol / liter were impregnated for 12, 24, and 36 hours, washed, dried, and then roasted at a temperature of 550°C; The mol / L nitric acid solution was treated at a temperature of 70°C for 5 hours, washed, dried, and then calcined at a temperature of 550°C to obtain the desired modified zeolite molecular sieve.

Embodiment 12

[0019] The modified zeolite molecular sieves prepared in Examples 1 to 11 and Comparative Example were measured on a Japan Rigaku D / max-1400 type X-ray diffractometer for XRD, and carried out a low-temperature nitrogen adsorption-desorption study on a TriStar3000 type physical adsorption instrument. The specific surface area of ​​the material is calculated by the BET method, and the pore size distribution and pore volume are calculated according to the BJH formula. The results are listed in Table 1 and Table 2.

[0020] Table 1 Nitrogen adsorption-desorption results

[0021] Example 1 2 3 4 5 6 acid exchange type hydrochloric acid hydrochloric acid hydrochloric acid nitric acid nitric acid nitric acid Acid exchange concentration / mol·liter -1 0.1 1.0 5.0 0.1 1.0 5.0 Acid exchange temperature / ℃ 20 50 90 90 50 20 Acid exchange time / hour 2 5 8 8 5 2 Types of pickling after alkali treatment hydrochloric acid ...

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Abstract

The invention relates to a method for preparing hollow cavity type ZSM-5 modified zeolite molecular sieve, and aims to solve the problems that the microcellular structure diffusion admittance is narrow, the modified zeolite molecular sieve has lower relative degree of crystallinity, and the adjustable range of apertures inside molecular sieve is small, thereby facilitating macromolecule reaction limited by diffusion. The invention adopts at least one 0.1-8.5 mol / L acid solution of hydrochloric acid, nitric acid, sulphuric acid or acetic acid to treat ZSM-5 molecular sieve raw powder with the silica alumina ratio SiO2 / Al2O3 being 20-1000 and the particle size being 0.4-10 Mum for 1-8 h; then at least one 0.1-5.0 mol / L aqueous alkali of sodium hydroxide, magnesium hydrate, potassium hydroxide, sodium carbonate or sodium bicarbonate is used for treatment for 1-48 h at 20-90 DEG C; and at least one 0.1-8.5 mol / L acid solution of hydrochloric acid, nitric acid, sulphuric acid or acetic acid is used for treatment for 1-48 h at 20-90 DEG C to obtain the modified ZSM-5 molecular sieve. The problems are well solved, and the invention can be used in industrial production of macromolecule catalysis and transformation catalysts.

Description

technical field [0001] The invention relates to a preparation method of a cavity type ZSM-5 modified zeolite molecular sieve. Background technique [0002] Zeolite molecular sieve materials have special shape-selective catalytic properties due to their uniform composition, regular structure, adjustable surface acidity and molecular size pore size. However, due to the limitation of its pore size, this kind of material is no longer suitable as a catalyst for reactions involving macromolecules, such as vacuum oil cracking with macromolecules. In 1992, researchers from Mobil Corporation in the United States successfully synthesized M41S series mesoporous molecular sieves, which have a large specific surface area, orderly arranged pores, and adjustable pore size distribution in the range of 2 to 10 nanometers, which can solve this problem (Kresge C T, Leonowivz M E , Roth W J, et al. Nature, 1992, 359: 710-712). However, due to the non-crystalline framework structure of M41S, i...

Claims

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Application Information

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IPC IPC(8): C01B39/38B01J29/40
Inventor 梅长松谢在库杨为民温鹏宇刘红星赵昱
Owner CHINA PETROLEUM & CHEM CORP
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