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Method for preparing ZSM-5 molecular sieve without template agent

A ZSM-5, template-free technology, applied in the field of molecular sieves, can solve the problems of high pressure, high crystallization temperature, and high production cost, and achieve the effects of high crystallinity, simplified process, and easy control of conditions

Active Publication Date: 2013-03-13
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Xiang Shouhe et al. of Nankai University (patent CN 1144191A) used NaZSM-5 with low silicon-aluminum ratio prepared by amine-free method as raw material, treated with inorganic acid or organic acid, and then crystallized at 400-800°C and 0.2-15MPa 1-6h, ZSM-5 with high silicon-aluminum ratio and high crystallinity is prepared. Its crystallization temperature is high and the pressure is high, so the preparation cost is high

Method used

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  • Method for preparing ZSM-5 molecular sieve without template agent
  • Method for preparing ZSM-5 molecular sieve without template agent
  • Method for preparing ZSM-5 molecular sieve without template agent

Examples

Experimental program
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Effect test

Embodiment 1

[0048] The main operation steps of this embodiment are as follows:

[0049] (1) Pulverize (ball mill) the gangue to d50=0.64μm, and then roast at 900°C for 2 hours.

[0050] (2) The roasted HCl solution with a concentration of 6mol / L, a solid-to-liquid ratio of 1:5, leached for 2 hours at 80°C, filtered and washed, and the obtained residual solid precursor SiO 2 / Al 2 o 3 The molar ratio was 21.

[0051] (3) Make a slurry mixture according to the following mass ratio, and acid-treat coal gangue (SiO 2 / Al 2 o 3 =21, with SiO 2 Molar ratio): NaOH: deionized water = 1: 0.15: 10, and then uniform refinement treatment.

[0052] (4) Put the homogeneously refined slurry in a reactor for crystallization reaction at 190°C for 72 hours. Filter and dry at 100°C for 12 hours to obtain ZSM-5. XRD results showed that the product was ZSM-5 phase with high crystallinity.

Embodiment 2

[0054] The main operation steps of this embodiment are as follows:

[0055] (1) Pulverize (ball mill) the coal gangue to d50=0.64μm, and then roast at 800°C for 2 hours.

[0056] (2) The roasted HCl solution with a concentration of 6mol / L, a solid-to-liquid ratio of 5.0, leaching at 90°C for 1 hour, filtered and washed, and the obtained residual solid precursor SiO 2 / Al 2 o 3 The molar ratio was 16.7.

[0057] (3) Make a slurry mixture according to the following mass ratio, and acid-treat coal gangue (SiO 2 / Al 2 o 3 =16.7, as SiO 2 Molar ratio): NaOH: deionized water = 1: 0.183: 11.67, and then uniform refinement treatment.

[0058] (4) The slurry obtained in step (3) was placed in a reactor at 190°C for crystallization reaction for 72 hours. Filter and dry at 100°C for 12 hours to obtain ZSM-5. XRD results show that the diffraction peaks are typical ZSM-5 diffraction peaks, and the crystallinity is high.

Embodiment 3

[0060] The main operation steps of this embodiment are as follows:

[0061] (1) Pulverize (ball mill) the gangue to d50=1.0μm, and then roast at 900°C for 2 hours.

[0062] (2) The roasted HCl solution with a concentration of 6mol / L, a solid-to-liquid ratio of 5.0, and 80°C were leached for 3 hours, filtered and washed to obtain the residual solid precursor SiO 2 / Al 2 o 3 The molar ratio was 22.4.

[0063] (3) Make a slurry mixture according to the following mass ratio, and acid-treat coal gangue (SiO 2 / Al 2 o 3 =22.4, as SiO 2 Molar ratio): NaOH: deionized water = 1: 0.15: 15, and then uniform refinement treatment.

[0064] (4) The slurry obtained in step (3) was placed in a reactor at 190°C for crystallization reaction for 72 hours. Filter and dry at 100°C for 12 hours to obtain ZSM-5. XRD results show that the diffraction peaks are typical ZSM-5 diffraction peaks, and the crystallinity is high.

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Abstract

The invention relates to a method for preparing a ZSM-5 molecular sieve without template agent. The method comprises the following steps of: smashing the mineral resource containing silicon oxide and aluminum oxide into powder, and roasting; leaching the roasted powder with acid liquor, regulating the amount of substance ratio of the silicon oxide to the aluminum oxide in solid phase to be (14:1)-(85:1), separating the solid phase, and removing impurities from the solid phase; mixing the obtained solid phase, the alkali and the water in the mass ratio of 1:(0.05-0.5):(5-30), carrying out hydrothermal reaction at 130-220 DEG C to crystallize for at least 18 hours, and removing impurities, thus obtaining the ZSM-5 molecular sieve. The method has the characteristics of adding no template agent, adding no additional silicon source or aluminum source, and saving the cost; the technology is simple to operate, the conditions are easy to control, and high value added utilization of waste resources is realized.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a method for preparing ZSM-5 molecular sieves without a template. Background technique [0002] ZSM-5 molecular sieve was first reported by Mobil in 1972. It is a five-membered ring zeolite. Its basic structural unit is composed of 8 five-membered rings. This basic structural unit is connected into a chain structure through oxygen bridges, and then It forms a zeolite framework and has a two-dimensional 10×10 ring channel structure (0.56nm×0.53nm and 0.55nm×0.51nm) (edited by Xu Ruren et al., Chemistry of Molecular Sieves and Porous Materials, 2004). The unique pore structure and acidity of ZSM-5 molecular sieve make it widely used as a shape-selective solid acid catalyst material in the deep processing of low-carbon olefins and aromatization, isomerization, alkylation, dealkylation, and substituted aromatics It shows unique performance in disproportionation and other reactions, e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 卢旭晨潘锋王体壮闫岩
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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