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A kind of synthetic method of multi-stage mesh molecular sieve

A network molecule and synthesis method technology, applied in the direction of molecular sieve compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of limited application, single mesoporous structure, low hydrothermal stability, etc., and achieve novel shape and shape The effect of high profile and profile hydrothermal stability

Active Publication Date: 2018-08-28
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the single mesoporous structure of mesoporous materials, its low hydrothermal stability and the characteristics of unidirectional pore system limit its application in industry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] The embodiment of the present invention provides a method for synthesizing a multi-stage mesh molecular sieve, comprising the steps of:

[0017] Add a certain amount of P123 into the dilute hydrochloric acid solution, add OP-10 and water in proportion, heat and stir in a water bath at a certain temperature, then add a certain amount of ethyl orthosilicate, continue stirring, and then add a certain amount of KF, Put it into a stainless steel reaction kettle, take it out and cool it after crystallization, filter it with suction, dry it to obtain a silicon-containing sample, and finally air roast it in a muffle furnace to obtain a white powder.

[0018] Among them, in this application document:

[0019] P123, Chinese name: polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, chemical formula PEO-PPO-PEO;

[0020] OP-10, Chinese name: alkylphenol polyoxyethylene ether;

[0021] Tetraethyl orthosilicate (TEOS), molecular formula Si(OC 2 h 5 ) 4 ...

Embodiment approach

[0024] Preferably, as an implementable mode, the method includes:

[0025] Step S110, dissolving P123 in dilute hydrochloric acid to form a first solution, taking OP-10 and dissolving it in water to form a second solution, mixing the first solution and the second solution, and stirring magnetically in a water bath at 36.5°C-37.5°C for 85 -95 minutes, then add ethyl orthosilicate and potassium fluoride to form the third solution, the consumption ratio of P123, OP-10, ethyl orthosilicate and potassium fluoride should make the mol ratio in the third solution be: OP- 10:P123:KF:SiO 2 :HCl:H 2 O=0.0085:0.017:0.01:1:5.8:197.

[0026] According to the above molar ratios, the proportions of P123, hydrochloric acid and other raw materials can be accurately obtained through calculation, and there are many ways to realize them, which are not listed in the embodiments of the present invention.

[0027] Step S111, after continuing to stir the third solution for 5.8-6.2 hours, put it int...

Embodiment 2

[0029] More preferably, as a preferred embodiment, the method includes the steps of:

[0030] Step S210, weigh 1g of P123 and dissolve it in 30ml of 2mol / L hydrochloric acid to form a first solution, then weigh 0.055g of OP-10 and dissolve it in 7.5ml of water to form a second solution, mix the two After mixing, stir magnetically in a water bath at 37°C for 1.5 h, then add 2.43 ml of ethyl orthosilicate and 0.01 g of potassium fluoride to form a third solution.

[0031] Step S211, after continuing to stir the third solution for 6 hours, put it into a stainless steel reaction kettle lined with polytetrafluoroethylene, crystallize at 100°C for 24 hours, cool at room temperature, wash with distilled water, and suction filter, Drying and calcining in air at 550° C. for 6 hours to obtain a multi-level mesh molecular sieve.

[0032] Throughout this article, unless otherwise specified, g is the unit of mass in gram, ml is the unit of volume in milliliter, h is the unit of time in ho...

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Abstract

The invention provides a method for synthesizing a multi-stage mesh molecular sieve, comprising the steps of dissolving P123 in dilute hydrochloric acid, dissolving OP-10 in water, mixing the two, and magnetic stirring in a water bath at 36.5°C-37.5°C , then add ethyl orthosilicate and potassium fluoride, continue to stir for 5.8-6.2 hours, put it into a stainless steel reaction kettle, crystallize at 95-105°C for 23.5-24.5 hours, cool at room temperature, filter with suction, and dry , 540°C-560°C air calcination for 5.8-6.2 hours to obtain a white powdery hierarchical porous network molecular sieve. The molecular sieve synthesized by the synthesis method provided by the invention has not single mesoporous structure, novel appearance and high hydrothermal stability.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for synthesizing a multi-stage mesh molecular sieve. Background technique [0002] Due to the single small pore size of microporous materials, the diffusion of molecules is limited, which seriously affects the application of zeolites in industrial catalysis. In order to overcome this problem, researchers have done a lot of work to expand the pore size of molecular sieves, thus discovering mesoporous materials. [0003] Mesoporous materials refer to a class of porous materials with pore sizes ranging from 2 to 50 nm. Mesoporous materials have the characteristics of extremely high specific surface area, regular and orderly pore structure, narrow pore size distribution, and continuously adjustable pore size, making it suitable for the adsorption and separation of macromolecules that are difficult for many microporous zeolite molecular sieves, especially ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B37/00
Inventor 马媛媛韩福忠邓庆芳贾丽华马凤延辛杨杨梦旸
Owner QIQIHAR UNIVERSITY
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