Preparation method of sodium-free fly ash-based ZSM-5 molecular sieve

A technology of ZSM-5 and fly ash, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of alkaline waste liquid discharge and cumbersome synthesis process, and achieve reduction Discharge of waste lye, wide range of sources of raw materials, and the effect of reducing discharge

Inactive Publication Date: 2019-08-23
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In summary, no matter which method is used to prepare ZSM-5 molecular sieve, the synthesis process will inevitably involve the conversion of silicon and aluminum into silicate and aluminate, which must be converted by adding a strong base, although the ZSM-5 molecular sieve that can be obtained -5 molecular sieve, but the synthesis process is relatively cumbersome, and the introduction of strong alkaline substances such as sodium hydroxide may cause the discharge of alkaline waste liquid

Method used

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  • Preparation method of sodium-free fly ash-based ZSM-5 molecular sieve
  • Preparation method of sodium-free fly ash-based ZSM-5 molecular sieve
  • Preparation method of sodium-free fly ash-based ZSM-5 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0022] First, take a certain amount of fly ash, ball mill it and then calcined to obtain calcined fly ash S 0 , then add distilled water and hydrochloric acid in the reaction kettle for 12 hours of hydrothermal reaction at 150°C, wash and dry to obtain acid-washed fly ash S 1 (mass ratio is M 蒸馏水 :M 粉煤灰 :M 盐酸 =1:0.5:2.5); take a certain amount of pickling fly ash S 1 , white carbon black, distilled water and tetrapropyl ammonium hydroxide (TPAOH) are placed in the reactor (mass ratio is M 白炭黑 : M 酸洗粉煤灰S1 =10:59), stirred for 2 hours, placed in a high-temperature oven at 180°C, crystallized for 48 hours, taken out, washed until neutral, dried, placed in a muffle furnace and calcined at 550°C for 5 hours to remove the template agent, and obtained ZSM-5 molecular sieve, denoted as FM-1. The ratio of the amount of material to be added is 200SiO 2 :1Al 2 o 3 :0.3TPAOH:20H 2 O.

Embodiment 2

[0024] First, take a certain amount of fly ash, ball mill it and then calcined to obtain calcined fly ash S 0 , then add distilled water and hydrochloric acid in the reaction kettle for 12 hours of hydrothermal reaction at 150°C, wash and dry to obtain acid-washed fly ash S 1 (mass ratio is M 蒸馏水 :M 粉煤灰 :M 盐酸 =1:0.5:2.5). Take a certain amount of pickling fly ash S 1 , white carbon black, distilled water and tetrapropyl ammonium hydroxide (TPAOH) are placed in the reactor (mass ratio is M 白炭黑 : M 酸洗粉煤灰S1=4:89), stirred for 2 hours, placed in a high-temperature oven at 180°C, crystallized for 48 hours, taken out, washed until neutral, dried, placed in a muffle furnace and calcined at 550°C for 5 hours to remove the template agent, and obtained ZSM-5 molecular sieve, denoted as FM-2. The ratio of the amount of material to be added is 100SiO 2 :1Al 2 o 3 :0.3TPAOH:20H 2 O.

Embodiment 3

[0026] First, take a certain amount of fly ash, ball mill it and then calcined to obtain calcined fly ash S 0 , then add distilled water and hydrochloric acid in the reaction kettle for 12 hours of hydrothermal reaction at 150°C, wash and dry to obtain acid-washed fly ash S 1 (The mass ratio is: M 蒸馏水 :M 粉煤灰 :M 盐酸 =1:0.5:2.5). Take a certain amount of pickling fly ash S 1 , silica sol (w=30%), distilled water and tetrapropyl ammonium hydroxide (TPAOH) are placed in the reactor (mass ratio is M 硅溶胶 :M 酸洗粉煤灰S1 =35:29), stirred for 2 hours, placed in a high-temperature oven at 180°C, crystallized for 48 hours, taken out, washed until neutral, dried, placed in a muffle furnace and calcined at 550°C for 5 hours to remove the template agent, and obtained ZSM-5 molecular sieve, denoted as FM-3. The ratio of the amount of material to be added is 100SiO 2 :1Al 2 o 3 :0.3TPAOH:20H 2 O.

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Abstract

The invention discloses a preparation method of a sodium-free fly ash-based ZSM-5 molecular sieve. The preparation method is characterized by comprising the following steps: a, carrying out ball milling on a certain amount of coal ash by using a ball mill, then fully carrying out calcining and activating by using a muffle furnace to obtain calcined fly ash without organic matter; b, adding a certain amount of distilled water and hydrochloric acid into the calcined fly ash, putting the mixture in a reaction kettle, carrying out a hydrothermal reaction, carrying out washing to neutrality, and carrying out drying to obtain acid-washed fly ash; and c, adding a silicon source into a certain amount of the acid-washed fly ash to adjust the silicon-aluminum ratio of the material, adding water anda template agent, and then carrying out a hydrothermal reaction to directly obtain the fly ash-based ZSM-5 molecular sieve which is free of strong alkali such as sodium hydroxide and the like by a one-step hydrothermal method. The fly ash with large reserves and wide sources is used for replacing expensive chemical reagents as raw materials to synthesize the ZSM-5 molecular sieve with high added value, so that difficulty of solid waste treatment is reduced, and meanwhile, a new idea is provided for synthesis of the ZSM-5 molecular sieve.

Description

technical field [0001] The invention relates to the field of inorganic catalyst materials, in particular to a method for preparing sodium-free ZSM-5 molecular sieves by calcining fly ash, pickling, and directly hydrothermally. [0002] technical background [0003] Since Landolt and Argauer first synthesized ZSM-5 zeolite molecular sieve in 1965, it has been widely used in industrial catalytic production because of its high specific surface area, adjustable pH, uniform micropore distribution and high thermal stability. The ZSM-5 molecular sieve has Z-shaped micropores of 0.55×0.51 nm on the [100] plane parallel to the a-axis, and a straight channel of 0.56×0.53 nm on the [010] plane parallel to the b-axis. Therefore, this structure can control the catalytic product to some extent by controlling the shape of the internal reaction space, thereby improving the catalytic selectivity of zeolites (YANG J, YU S, HU H, et al. Synthesis of ZSM-5 hierarchical microsphere-like particle ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03
Inventor 杨世诚张玉龙薛晓晓孙琦谌伦建
Owner HENAN POLYTECHNIC UNIV
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