Method of using gangue to prepare high purity molecular sieve ZSM-5

A ZSM-5, coal gangue technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of not yet high-purity molecular sieve, etc., to reduce the preparation cost and ease the operating conditions. , the effect of high purity

Inactive Publication Date: 2016-12-14
INNER MONGOLIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, some research groups have successfully prepared A-type molecular sieves, X-type molecular sieves, and Y-type molecular sieves using coal gangue as raw materials, but there is no report on the preparation of high-purity molecular sieve ZSM-5 using coal gangue as raw materials.

Method used

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  • Method of using gangue to prepare high purity molecular sieve ZSM-5
  • Method of using gangue to prepare high purity molecular sieve ZSM-5

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The coal gangue was roasted and activated at 850°C for 5 hours, and 25 g of the roasted coal gangue was weighed, treated with 6 mol / L hydrochloric acid for 4 hours, then filtered with deionized water, washed until neutral and dried; the dried samples were placed in Put into 5mol / I NaOH alkali solution, react under high temperature and high pressure for 3h (temperature is 160°C, pressure is 0.5MPa); after the reaction is completed, take 10mL of the reaction solution, adjust its pH value to 10.0 with hydrochloric acid; add 1.864g of tetrapropane Ammonium bromide (TPABr) and stirred for 12 hours, then transferred to a polytetrafluoroethylene reactor for hydrothermal reaction at 180°C for 24 hours, filtered, washed, dried, and roasted at 550°C for 4 hours in a muffle furnace to obtain high-purity molecular sieve ZSM -5.

Embodiment 2

[0024] The coal gangue was roasted and activated at 850°C for 5 hours, and 25 g of the roasted coal gangue was weighed, treated with 6 mol / L hydrochloric acid for 4 hours, then filtered with deionized water, washed until neutral and dried; the dried samples were placed in Add 8mol / L NaOH alkali solution, react under normal temperature and pressure for 3 days; After the reaction is completed, get the reaction solution 10mL, adjust its pH value at 10.0 with hydrochloric acid; add 1.864g of tetrapropylammonium bromide (TPABr) and stir After 12 hours, it was transferred to a polytetrafluoroethylene reactor for hydrothermal reaction at 180°C for 24 hours, filtered, washed, dried, and then roasted in a muffle furnace at 550°C for 4 hours to obtain high-purity molecular sieve ZSM-5.

Embodiment 3

[0026] The coal gangue was roasted and activated at 850°C for 5 hours, and 25 g of the roasted coal gangue was weighed, treated with 6 mol / L hydrochloric acid for 4 hours, then filtered with deionized water, washed until neutral and dried; the dried samples were placed in Put into 5mol / L NaOH alkali solution, react under high temperature and high pressure for 3h (temperature is 160°C, pressure is 0.5MPa); after the reaction is completed, take 10mL of the reaction solution, adjust its pH value to 10.0 with hydrochloric acid; add 1.864g of tetrapropane Ammonium bromide (TPABr) and stirred for 12 hours, then transferred to a polytetrafluoroethylene reactor for hydrothermal reaction at 140°C for 48 hours, filtered, washed, dried, and then roasted in a muffle furnace for 4 hours at 550°C to obtain high-purity molecular sieve ZSM -5.

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Abstract

The invention discloses a method of using gangue to prepare a high purity molecular sieve ZSM-5. The method comprises the following steps: taking gangue as the raw material, burning gangue to activate gangue, soaking gangue in acid, then adding an alkali solution with a certain concentration, carrying out reactions under a high pressure at a high temperature to obtain a silicon-aluminum source, adjusting the pH value of the obtained silicon-aluminum source to a certain range, adding a surfactant (tetrapropyl ammonium bromide), stirring for a while at a room temperature, then carrying out reactions at a temperature of 120 to 180 DEG C for 12 to 48 hours under hydrothermal conditions, filtering, washing, drying, and burning to obtain the high purity molecular sieve ZSM-5. The solid waste gangue is taken as the raw material to synthesize the high purity molecular sieve ZSM-5, the raw material is cheap and easily available, the operation conditions are not strict, and the purity of the prepared molecular sieve ZSM-5 is high.

Description

technical field [0001] The invention relates to a method for preparing molecular sieves, in particular to a method for preparing high-purity molecular sieve ZSM-5 by using coal gangue. Background technique [0002] Molecular sieve ZSM-5 is a new structure zeolite molecular sieve with high silicon three-dimensional crossed straight channels first developed by Mobile Company of the United States in 1972. The molecular sieve has a pore size distribution of 0.55nm, is lipophilic and hydrophobic, has excellent thermal stability, acid stability and catalytic activity, and also has good hydrophobicity and hydrothermal stability. Because of its unique pore structure, it has become One of the most important catalytic materials in field shape-selective reactions. [0003] At present, the silicon and aluminum sources used in the preparation of ZSM-5 are mostly existing chemical reagents, such as tetraethyl orthosilicate (TEOS), methyl orthosilicate (TMOS), sodium silicate and aluminum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
CPCC01B39/38C01P2002/72C01P2004/03
Inventor 杜春芳刘晓艳刘志亮
Owner INNER MONGOLIA UNIVERSITY
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