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Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve

A technology of zeolite molecular sieve and fly ash, which is applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of difficult activation of silicon-alumina in the crystal phase, complex multi-level porosity process, and product Poor crystallinity and other problems, to achieve the effect of easy operation, avoiding high energy consumption and saving energy

Inactive Publication Date: 2021-01-08
GUIZHOU INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the deficiencies of the prior art, the present invention provides a preparation method of fly ash-based microporous and multi-stage zeolite molecular sieves, which solves the defects existing in the prior art, such as difficult activation of crystalline phase silicon-aluminum species or activation energy Problems such as high energy consumption, complex multi-stage porosity process, and poor product crystallinity

Method used

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  • Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve
  • Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve
  • Preparation method of fly ash-based microporous and hierarchical porous zeolite molecular sieve

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Embodiment 1

[0039]The fly ash was selected from Zhenyuan County, Guizhou, and its chemical composition is shown in Table 1; the ICP test results of the precursor fluid are shown in Table 2.

[0040] 1) Get fly ash and carry out ball milling, and cross 900 mesh sieves;

[0041] 2) According to the liquid-solid ratio (mL:g) of 10, add 200mL of sodium hydroxide solution with a concentration of 4mol / L into the special-shaped three-necked flask, and add 20g of fly ash after ball milling and sieving;

[0042] 3) Place the above-mentioned three-necked bottle in a microwave-ultrasonic-ultraviolet light combined catalytic synthesizer, place an immersion ultrasonic alloy probe on the top port, ultrasonic power 20KHz, and ultrasonically treat the mixture for 40 minutes;

[0043] 4) Set the temperature of the reactor to 100°C, and the microwave treatment time is 2 hours. The microwave module automatically outputs according to the power of 0-1000W, and the ultrasound continues to act for 2 hours; the ...

Embodiment 2

[0055] The fly ash was selected from Zhenyuan County, Guizhou Province, and its chemical composition is shown in Table 1; the ICP test results of the precursor fluid are shown in Table 3.

[0056] 1) Get fly ash and carry out ball milling, and cross 900 mesh sieves;

[0057] 2) According to the liquid-solid ratio (mL:g) of 5, add 200mL of sodium hydroxide solution with a concentration of 4mol / L into the special-shaped three-necked flask, and add 40g of fly ash after ball milling and sieving;

[0058] 3) Place the above-mentioned three-necked bottle in a microwave-ultrasonic-ultraviolet light combined catalytic synthesizer, place an immersion ultrasonic alloy probe on the top port, ultrasonic power 20KHz, and ultrasonically treat the mixture for 40 minutes;

[0059] 4) Set the temperature of the reactor to 100°C, and the microwave treatment time is 2 hours. The microwave module automatically outputs according to the power of 0-1000W, and the ultrasound continues to act for 2 ho...

Embodiment 3

[0069] The fly ash was selected from Jinsha County, Guizhou Province, and its chemical composition is shown in Table 4; the ICP test results of the precursor fluid are shown in Table 5.

[0070] 1) Get fly ash and carry out ball milling, and cross 900 mesh sieves;

[0071] 2) According to the liquid-solid ratio (mL:g) of 15, add 200 mL of sodium hydroxide solution with a concentration of 5 mol / L into the special-shaped three-necked flask, and add 13.33 g of fly ash after ball milling and sieving;

[0072] 3) Place the above-mentioned three-necked bottle in a microwave-ultrasonic-ultraviolet light combined catalytic synthesizer, place an immersion-type ultrasonic alloy probe on the top port, ultrasonic power 25KHz, and ultrasonically treat the mixture for 20 minutes;

[0073] 4) Set the temperature of the reactor to 110°C, and the microwave treatment time is 1 hour. The microwave module automatically outputs according to the power of 0-1000W, and the ultrasound continues to act...

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Abstract

The invention discloses a green preparation method of a fly ash-based microporous and hierarchical porous zeolite molecular sieve, wherein the method comprises the steps: mixing a sodium hydroxide solution and fly ash, replacing a traditional high-energy consumption alkali fusion technology with a microwave-ultrasonic-ultraviolet light synergistic activation technology, efficiently extracting silicon-aluminum components and residual carbon particles in the fly ash, and thus obtaining high-purity aluminosilicate precursor solution; supplementing an aluminum source or a structure directing agentor deionized water into the precursor solution, marking the aluminosilicate precursor solution as a solution A1, adding a tetrapropylammonium hydroxide solution into the solution A1, marking the mixed solution as a solution A2, dissolving sodium metaaluminate into the deionized water, marking the solution as a solution B, dropwise adding the solution B into the solution A1, and stirring to obtaina solution C; and putting one of the solution A1, the solution A2 and the solution C into a lining of a high-pressure reaction kettle to react, carrying out suction filtration on materials in the kettle after the reaction, washing until the pH value is neutral, drying and roasting to obtain a solid product. The method has the advantages of avoiding of an impurity removal process, simplification of a multistage porification process, simplicity and convenience in operation, short reaction time, energy saving and high purity of the obtained product.

Description

technical field [0001] The invention relates to the technical field of fly ash recycling, in particular to a green preparation method of fly ash-based microporous and multi-stage zeolite molecular sieves. Background technique [0002] Zeolite molecular sieve is a kind of hydrated aluminosilicate crystal. There are many pores with uniform pore size and neatly arranged cavities in the skeleton structure. It is widely used as industrial catalyst, ion exchanger, adsorption and separation in petrochemical, fine chemical and other fields. detergents and detergents, etc. The cost of synthesizing zeolite molecular sieves with pure industrial raw materials is relatively high, and the main component of fly ash is the main raw material for synthesizing zeolite molecular sieves SiO 2 and Al 2 o 3 , Using fly ash instead of pure industrial raw materials can not only save production costs, but also turn waste into treasure and realize the recycling of solid waste. [0003] In addition...

Claims

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Application Information

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IPC IPC(8): C01B39/48C01B39/04
CPCC01B39/04C01B39/48C01P2002/72C01P2004/03C01P2006/12C01P2006/14C01P2006/17
Inventor 宋国强陈文婷
Owner GUIZHOU INST OF TECH