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Improved silicon source used for zeolite molecular sieve and prepared by enhanced dissolution method

A technology of zeolite molecular sieve and silicon source, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of increasing solvent consumption, energy consumption and processing costs, and poor stability of high-concentration solutions In order to achieve the effect of simple preparation method and high efficiency

Active Publication Date: 2021-06-08
SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This obviously significantly increases solvent usage, energy consumption and disposal costs
However, the idea of ​​using soluble silicon materials such as organic silicon to prepare a high-concentration silicon solution is limited by the poor stability of the high-concentration solution, which makes the silicon material easy to gel, settle and precipitate.
In addition, the chemical composition of the silicon solution configured with organic silicon and other materials is obviously more complex, and it is difficult to use it as a raw material for the preparation of zeolite molecular sieves

Method used

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  • Improved silicon source used for zeolite molecular sieve and prepared by enhanced dissolution method
  • Improved silicon source used for zeolite molecular sieve and prepared by enhanced dissolution method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Soak the dense silicon source pectate silicon soaked in the rod water, 38% concentrated hydrochloric acid or 68% concentrated nitric acid solution, soaking time is 12 hours.

[0051] (2) The mixture in (1) is grinded in a high energy ball mill, and the rotational speed is 1500R / min, the ball ratio 10: 1, the grinding time is 8 hours.

[0052] (3) The aqueous solution of methanol is formulated, and the potassium hydroxide is added to 14, and the silicon feedstock treated by step (2) is transferred to a water heat synthetic kettle, under temperature conditions of 180 ° C, in the base methanol The aqueous solution was dissolved for 5 hours.

[0053] (4) The formulated concentration ranges from 0.1 mol / L of potassium bromide aqueous solution, and mixed with silicon (3) under high strength agitation conditions under high strength stirring conditions.

[0054] (5) Spray the stabilized mixed solution prepared in (4) to spray the coating machine on the hot metal plate. The ...

Embodiment 2

[0057] Step (1) use 1 mol / L of more dilute hydrochloric acid or nitric acid, soaking on impurity removal on impurities within one day, the soaking time needs to be extended to 3 days. Other operations are the same as in Example 1 (2-5) or (2-6), and an approximate effect can also be obtained.

Embodiment 3

[0059] Step (5) The effect of using freeze-drying (-20 ° C overnight dry) is slightly in spray drying, and the silicon material is slightly agglomerated, but can be promoted in step (6).

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Abstract

The invention relates to a dominant silicon source prepared by an enhanced dissolution method and an ultra-small zeolite molecular sieve nanocrystal prepared by using the silicon source, and particularly discloses a preparation method of the silicon source. The preparation method comprises the following steps: 1) soaking a compact silicon source in an acid solution to remove impurities; 2) crushing a material obtained in the step 1) through ball milling; 3) preparing an aqueous solution of methanol, adjusting a pH value to 12-14, adding the ball-milled and crushed silicon material, and dissolving the silicon material at 100-300 DEG C by using a solvothermal method to obtain a silicon solution; 4) preparing an alkali metal source solution, and mixing the alkali metal source solution with the silicon solution obtained in the step 3); 5) rapidly and uniformly removing the solvent to obtain a silicon-alkali metal binary uniformly-embedded mixture; and 6) with the silicon-alkali metal binary uniformly-embedded mixture prepared in the step 5) as an improved silicon source for synthesis of the zeolite molecular sieve, and crystallizing the improved silicon source and other components required by synthesis. Thus, a crystallization rate can be increased, and an ultra-small nanocrystal product of the zeolite molecular sieve can be obtained.

Description

Technical field [0001] The present invention belongs to the field of zeolite molecular sieves, and more particularly to an advantageous silicon source prepared by reinforced dissolution method, and a zeolite molecular sieve super small nanocrystals prepared using this silicon source. Background technique [0002] The zeolite molecular sieve has a wide range of industrial applications involving all aspects of production. In many applications, zeolite molecular sieves with particle diameter at 100 nm or less often have obvious properties of ordinary crystals, and even reflecting some of ordinary crystals do not have performance, so that the preparation of ultra-small nano-crystals has always been zeolite molecular sieves. Long-term research hotspots in the field of research. However, due to the high technical difficulty, only 20 of the 250 zeolite molecular sieve structures have been reported, only 20 nanocrystals [1] of 100 nm or less, and the zeolite material below 20 nm is more ...

Claims

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Application Information

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IPC IPC(8): C01B39/02C01B39/04
CPCC01B39/02C01B39/026C01B39/04C01P2004/03
Inventor 喻学锋李睿黄逸凡康翼鸿高明
Owner SHENZHEN INST OF ADVANCED TECH CHINESE ACAD OF SCI
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