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Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash

A technology of ZSM-5 and fly ash, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problem of high production cost of ZSM-5 molecular sieve, and achieve high-value utilization, Lower synthesis cost and better crystallinity

Inactive Publication Date: 2013-12-11
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] An object of the present invention is to provide the method utilizing fly ash to prepare nanoscale ZSM-5 molecular sieve, it is used to solve the higher problem of ZSM-5 molecular sieve production cost

Method used

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  • Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash
  • Method for preparing nano-scale ZSM-5 molecular sieve by using coal ash

Examples

Experimental program
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Effect test

Embodiment 1

[0025] combine figure 2 , take fly ash collected on site as raw material, grind it into fine powder, pass through a 200-mesh sieve, take 100g of fine powder and place it in a muffle furnace, calcinate at 800°C for 2 hours, then burn it at a temperature of 75°C and a speed of 250r / Min was washed twice with water for 0.5 hours each time, and then the washing liquid was separated from the fly ash for solid-liquid separation. After separation, the solid was dried at 120°C for 5 hours for later use; the pretreated fly ash was mixed with Na 2 CO 3 The mass ratio of solids is 1:1 and mixed evenly. After roasting at 800°C for 2 hours, take it out and cool it to 25°C for later use; then impregnate the roasted product with 3mol / L HCl for 60 minutes, filter to remove insoluble matter, and obtain silica-rich gel and crude AlCl 3 solution. Adjust crude AlCl with 4% NaOH 3 pH value of the solution to 3.5, filtered to remove Fe(OH) 3 , the filtrate continued to add NaOH dropwise until...

Embodiment 2

[0027] Use fly ash collected on site as raw material, grind it into fine powder, pass through a 200-mesh sieve, put 100g of fine powder in a muffle furnace, calcinate at 750°C for 3 hours, then wash with water at 50°C and 200r / min for 2 hours time, 1 hour each time, and then carry out solid-liquid separation between the washing solution and the fly ash, and dry the solid at 120°C for 5 hours after separation; the pretreated fly ash and Na 2 CO 3 The mass ratio of solids is 1:1.2 and mixed evenly. After roasting at 750°C for 2.5 hours, take it out and cool it to 25°C for later use; then impregnate the roasted product with 2.5mol / L HCl for 70 minutes, filter to remove insoluble matter, and obtain silicon-rich gel and Crude AlCl 3 solution. Adjust crude AlCl with 8% NaOH 3 pH value of the solution to 3, filtered to remove Fe(OH) 3 , the filtrate continued to add NaOH dropwise until the precipitation in the filtrate no longer increased, and the Mg(OH) was removed by filtration...

Embodiment 3

[0029] Use fly ash collected on site as raw material, grind it into fine powder, pass through a 200-mesh sieve, put 100g of fine powder in a muffle furnace, calcinate at 750°C for 3 hours, then wash with water at 50°C and 200r / min for 2 hours time, 1 hour each time, and then carry out solid-liquid separation between the washing solution and the fly ash, and dry the solid at 120°C for 5 hours after separation; the pretreated fly ash and Na 2 CO 3 The mass ratio of solids is 1:1.2 and mixed evenly. After roasting at 750°C for 2.5 hours, take it out and cool it to 25°C for later use; then impregnate the roasted product with 2.5mol / L HCl for 70 minutes, filter to remove insoluble matter, and obtain silicon-rich gel and Crude AlCl 3 solution. Adjust crude AlCl with 8% NaOH 3 pH value of the solution to 3, filtered to remove Fe(OH) 3 , the filtrate continued to add NaOH dropwise until the precipitation in the filtrate no longer increased, and the Mg(OH) was removed by filtration...

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Abstract

The invention relates to a method for preparing a nano-scale ZSM-5 molecular sieve by using coal ash. The method comprises the following steps: pre-treating coal ash; using the coal ash subjected to pretreatment to prepare aluminum hydroxide and sodium silicate; uniformly mixing the aluminum hydroxide and the sodium silicate which are obtained after the coal ash is processed with water and the template agent tetrapropyl-ammonium hydroxide, wherein molar fraction of the water, the tetrapropyl-ammonium hydroxide, the aluminum hydroxide and the sodium silicate are respectively 90-98 percent, 0.25-1.0 percent, 0.025-0.01 percent and 1-2 percent; performing microwave auxiliary synthesis for 24-72 hours at the temperature of 150-250 DEG C; taking out a product in a reaction kettle, washing for 2-5 times with water at the temperature of 60-80 DEG C, and drying at the temperature of 120 DEG C for 12-24 hours; after drying, roasting the product at the temperature of 600-800 DEG C for 4-8 hours to obtain a nano-scale ZSM-5 molecular sieve finished product, wherein the particle size of the ZSM-5 molecular sieve is 200-500 nm. According to the method, the synthesis cost of the ZSM-5 molecular sieve is reduced, the problem of environment pollution caused by coal ash is reduced, and high-value use of the coal ash is realized.

Description

1. Technical field: [0001] The invention relates to a method for preparing ZSM-5 molecular sieves in the field of petrochemical industry, in particular to a method for preparing nanometer ZSM-5 molecular sieves by using fly ash. 2. Background technology: [0002] ZSM-5 molecular sieve was first successfully developed by Mobil Company of the United States in 1972 (US3702886). It is an aluminosilicate zeolite molecular sieve with a high silicon-aluminum ratio and a three-dimensional straight-through pore structure. It is mainly composed of Si-O and Al-O tetrahedrals. body, and connected into straight channels and sinusoidal channels with evenly distributed pore diameters. ZSM-5 molecular sieve has a large number of holes in the crystal structure, and movable water molecules and cations are distributed in the holes. Since it has no cage, it is not easy to deposit carbon during the catalytic process, and has good thermal stability and acid resistance. properties, hydrophobicity...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00
Inventor 韩洪晶陈彦广陆佳宋华解骢浩徐婷婷
Owner NORTHEAST GASOLINEEUM UNIV
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