A zeolite molecular sieve modified silicon source 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 The problem of high efficiency and simple preparation method can be achieved by solving the problems of non-resistance, difficult zeolite molecular sieve preparation raw materials and other problems.

Active Publication Date: 2022-08-05
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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  • A zeolite molecular sieve modified silicon source prepared by enhanced dissolution method
  • A zeolite molecular sieve modified silicon source prepared by enhanced dissolution method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Soak the dense silicon source dry colloidal silicon in aqua regia, 38% concentrated hydrochloric acid or 68% concentrated nitric acid solution for 12 hours.

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

[0052] (3) prepare the aqueous solution of methanol, add potassium hydroxide to adjust the pH value to 14, transfer the silicon raw material processed in step (2) to the hydrothermal synthesis kettle, under the temperature condition of 180 ℃, in alkaline methanol Dissolved in aqueous solution for 5 hours.

[0053] (4) A potassium bromide aqueous solution with a concentration range of 0.1 mol / L is prepared, and is added dropwise and mixed with the silicon solution in (3) under high-intensity stirring conditions.

[0054] (5) The stable mixed solution prepared in (4) was sprayed on the hot metal plate using a coating machine. The tempera...

Embodiment 2

[0057] In step (1), 1 mol / L of relatively dilute hydrochloric acid or nitric acid is used, and the effect of soaking within one day on the removal of impurities is limited, and the soaking time needs to be extended to about 3 days. Other operations are the same as (2-5) or (2-6) in Example 1, and similar effects can also be obtained.

Embodiment 3

[0059] The effect of freeze drying (-20°C overnight drying) in step (5) is slightly inferior to spray drying, and the silicon material has a slight self-agglomeration phenomenon, but it can still play a promoting role in step (6).

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Abstract

The invention relates to a superior silicon source prepared by an enhanced dissolution method, and ultra-small nanocrystals of zeolite molecular sieve prepared by using the silicon source, and specifically discloses a preparation method thereof, including 1) immersing a dense silicon source in an acid solution to remove impurities; 2. ) crushing the material obtained in step 1) by ball milling; 3) preparing an aqueous solution of methanol, adjusting the pH value to 12-14, adding the silicon material crushed by ball-milling, and dissolving by solvothermal method at 100-300° C. to obtain a silicon solution; 4) prepare an alkali metal source solution and mix with the silicon solution in (3); 5) remove the solvent quickly and uniformly to obtain a silicon-alkali metal binary uniform embedding mixture; 6) use the silicon-alkali metal prepared in (5) The alkali metal binary homogeneous intercalation mixture is used as an improved silicon source for the synthesis of zeolite molecular sieves, and it can be crystallized with other components required for the synthesis, which can improve the crystallization rate and obtain ultra-small nanocrystalline products of zeolite molecular sieves.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, and in particular relates to an advantageous silicon source prepared by an enhanced dissolution method, and ultra-small nanocrystals of zeolite molecular sieve prepared by using the silicon source. Background technique [0002] Zeolite molecular sieves have a wide range of industrial applications, involving all aspects of production and life. In many application fields, ultra-small nanocrystals of zeolite molecular sieves with a particle size of less than 100 nm often have significantly better properties than ordinary crystals, and even show some properties that ordinary crystals do not have. Therefore, the preparation of ultra-small nanocrystals has always been a zeolite molecular sieve. A long-term research hotspot in the research field. However, due to the great technical difficulty, among the 250 zeolite molecular sieve structures reported so far, only about 20 have...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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