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Microwave assisted method for synthesizing CHA molecular sieve from gangue

A microwave-assisted, coal gangue technology, which is applied in the fields of resource utilization and energy saving and emission reduction, can solve the problems of high preparation cost, environmental pollution, and long synthesis time of SSZ-13, so as to reduce synthesis time and preparation cost and improve utilization The effect of high efficiency and high output

Active Publication Date: 2017-02-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the current problems of sharp increase in coal gangue output, low utilization rate, pollution to the environment, high preparation cost and long synthesis time of SSZ-13, the present invention provides a method for synthesizing CHA from coal gangue assisted by microwaves, which not only improves the utilization of coal gangue efficiency, reducing environmental pollution, while improving the crystallinity and uniformity of SSZ-13 zeolite, effectively reducing its synthesis time and preparation cost, and laying the foundation for the industrial production and large-scale application of SSZ-13

Method used

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  • Microwave assisted method for synthesizing CHA molecular sieve from gangue
  • Microwave assisted method for synthesizing CHA molecular sieve from gangue
  • Microwave assisted method for synthesizing CHA molecular sieve from gangue

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Experimental program
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Effect test

Embodiment 1

[0032] Embodiment 1: a kind of method for microwave-assisted coal gangue synthesis CHA molecular sieve, concrete steps are as follows:

[0033] Step 1: pulverizing and grinding the coal gangue, and passing through a 200-mesh sieve to obtain coal gangue powder with uniform particle size;

[0034] Step 2: Take 0.1762g KOH solid and dissolve it in 26.1832g distilled water (that is, the molar concentration of the KOH solution is 0.12mol / L), and after the KOH solid is completely dissolved, add 0.2001g of coal gangue powder with a silicon-aluminum molar ratio of 2.0 (over 200 Mesh sieve), after stirring for 60min, mixed solution A was obtained;

[0035] Step 3: Add 6.3252 g of N,N,N-trimethyl-1-adamantyl ammonium hydroxide with a mass fraction of 25% to the mixed solution A obtained in Step 2, and continue stirring for 60 minutes to obtain a mixed solution B;

[0036] Step 4: Add 1.1320g of white carbon black to the mixed solution B obtained in Step 3, and continue to stir for 60mi...

Embodiment 2

[0039] Embodiment 2: A method for synthesizing CHA molecular sieves from microwave-assisted coal gangue. The basic steps are the same as in Embodiment 1. The difference is that in step 5, the crystallization time is changed from 12h to 18h, and the obtained crystal structure is better after filtering, drying and roasting. SSZ-13 type molecular sieve.

[0040] Depend on figure 1 Comparing the XRD patterns of standard and 2, it can be seen that the molecular sieve synthesized in Example 2 belongs to the pure phase CHA type zeolite molecular sieve. According to FIG. 3(B), it can be seen that the crystallization effect of the molecular sieve prepared in Example 2 is better, and the crystal block is relatively uniform.

[0041] According to Examples 1 and 2, it can be seen that as the crystallization time increases, the amorphous state of the synthesized SSZ-13 gradually decreases, and the crystal structure gradually becomes better.

Embodiment 3

[0042] Embodiment three: a kind of method for microwave-assisted gangue synthesis CHA molecular sieve, basic steps are the same as embodiment one, difference is: the molar concentration of KOH solution in step two becomes 0.5mol / L by 0.12mol / L, stirring time Changed from 60 min to 90 min; in step five, the crystallization temperature was changed from 160°C to 180°C, and finally an SSZ-13 analytical sieve with a better crystal structure was obtained.

[0043] Depend on figure 2 Comparing the XRD patterns of standard and 3, it can be seen that the molecular sieve synthesized in Example 3 belongs to the pure phase CHA type zeolite molecular sieve. Fig. 3 (C) is a relatively pure cubic block, illustrating that the crystallization effect of the molecular sieve synthesized in Example 3 is better.

[0044]According to 1 and 3, it can be seen that increasing the concentration of KOH solution, prolonging the stirring time, and increasing the crystallization temperature can reduce the...

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Abstract

The invention discloses a microwave assisted method for synthesizing CHA molecular sieve from gangue. The method comprises the following steps: adding gangue powder to a prepared KOH solution, and stirring the gangue powder and the prepared KOH solution for a period of time; adding N,N,N-trimethyl-1-adamantanaminium hydroxide to the above obtained mixed solution, and stirring for a period of time; adding silica sol or white carbon black used as a silicon source, and continuously stirring for a period of time; and transferring the above obtained mixture into a microwave heating reaction kettle, carrying out a crystallization reaction, carrying out room temperature cooling, washing the obtained solid phase product with deionized water, filtering the washed solid phase product, drying the filtered solid phase product, and roasting the dried solid phase product in air at 450-600 DEG C in order to obtain SSZ-13 molecular sieve. The gangue used in the invention belongs to solid wastes generated in the coal chemical industry, so the current theme of changing of wastes into valuables, energy saving and environmental protection are met; and the microwave assisted synthesis method greatly shortens the synthesis time of the SSZ-13, improves the crystal performances and the crystal grain uniformity of the SSZ-13, promotes the solid phase yield of the SSZ-13, and is in favor of realizing large-scale production and industrial application of the SSZ-13.

Description

technical field [0001] The invention relates to a method for synthesizing CHA molecular sieves from coal gangue assisted by microwaves, and belongs to the fields of resource utilization and energy saving and emission reduction. Background technique [0002] Coal gangue is one of the main solid wastes produced during coal mining. With the continuous expansion of coal production, the production of coal gangue is increasing day by day. The utilization of coal gangue in my country started late, the comprehensive utilization rate is low, and the equipment technology is backward. As a result, the long-term stacking and capture of coal gangue occupies land and pollutes water sources, soil and air around mining areas. , and even seriously damaged the ecological environment and ecological landscape of the mining area. At present, the utilization of coal gangue is mainly concentrated in the fields of engineering fillers, power generation, building materials products, etc., and the tec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72
Inventor 刘庆岭韩金峰赵倩葛云丽晋晓彤纪娜宋春风
Owner TIANJIN UNIV