A high-efficiency synthesis method of dual-silicon source and amine-free large-size mordenite with controllable morphology

A technology of mordenite and synthesis method, applied in the direction of mercerized crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve problems such as complex operation process, long crystallization time of ordinary mordenite, environmental pollution, etc., and achieve separation process The effect of simple operation, convenient recycling of catalytic application, and simple and easy operation

Inactive Publication Date: 2017-03-22
SHANDONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are many problems in the synthesis process of mordenite in the prior art. (1) Most of the synthesis of mordenite will rely on organic amines, inorganic ammonia or fluorides as templates, which are very easy to pollute the environment; (2) The crystallization time of ordinary mordenite is long, and the crystallization time is generally more than 24h. Although large-size mordenite can be synthesized, the crystallization time of large-size mordenite crystals is often more than 3-8 days; (3) preparing large-size mordenite crystals Zeolite is commonly used with organic substances such as alcohols, and the operation process is complicated

Method used

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  • A high-efficiency synthesis method of dual-silicon source and amine-free large-size mordenite with controllable morphology
  • A high-efficiency synthesis method of dual-silicon source and amine-free large-size mordenite with controllable morphology
  • A high-efficiency synthesis method of dual-silicon source and amine-free large-size mordenite with controllable morphology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Water glass is carried out pretreatment, gets 0.32g sodium hydroxide (96wt% NaOH), 0.82g sodium aluminate (41wt% Al 2 o 3 ) was dissolved in 5g deionized water, and the resulting solution was added dropwise to 103.82g water glass (14.74wt% SiO 2 , 5.22 wt% Na 2 O), mechanically stirred for 1 h to obtain a suspension, which was set aside.

[0034] Dissolve 0.59g of sodium hydroxide and 0.79g of sodium aluminate in 30.22g of deionized water, add the suspension aged for 24 hours to the obtained transparent solution, stir mechanically for 0.5 hours, and then add dropwise 15.79g of orthosilicon Ethyl acetate, so that the SiO of two silicon sources (treated water glass and tetraethyl orthosilicate) 2 The molar ratio is 0.83:1, and mechanically stirred for 2 hours to obtain the initial gel of mordenite, wherein the material molar ratio is: 35SiO 2 : 1.17Al 2 o 3 : 10Na 2 O: 750H 2 O. After aging for 24 hours, it was transferred to a polytetrafluoroethylene-lined autoc...

Embodiment 2

[0036] Water glass is carried out pretreatment, gets 0.32g sodium hydroxide (96wt% NaOH), 0.82g sodium aluminate (41wt% Al 2 o 3 ) was dissolved in 5g deionized water, and the resulting solution was added dropwise to 103.82g water glass (14.74wt% SiO 2 , 5.22 wt% Na 2 O), mechanically stirred for 1 h to obtain a suspension, which was set aside.

[0037]Dissolve 0.76g of sodium hydroxide and 0.84g of sodium aluminate in 43.44g of deionized water, add the suspension aged for 24 hours to the obtained transparent solution, stir mechanically for 0.5 hours, and then add dropwise 15.79g of orthosilicon Ethyl acetate, so that the SiO of two silicon sources (treated water glass and tetraethyl orthosilicate) 2 The molar ratio is 0.50:1, and mechanically stirred for 2 hours to obtain the initial gel of mordenite, wherein the material molar ratio is: 35SiO 2 : 1.17Al 2 o 3 : 10Na 2 O: 750H 2 O. After aging for 24 hours, it was transferred to a polytetrafluoroethylene-lined autocl...

Embodiment 3

[0039] Water glass is carried out pretreatment, gets 0.32g sodium hydroxide (96wt% NaOH), 0.82g sodium aluminate (41wt% Al 2 o 3 ) was dissolved in 5g deionized water, and the resulting solution was added dropwise to 103.82g water glass (14.74wt% SiO 2 , 5.22 wt% Na 2 O), mechanically stirred for 1 h to obtain a suspension, which was set aside.

[0040] Dissolve 1.23g of sodium hydroxide and 0.58g of sodium aluminate in 30.22g of deionized water, add the suspension aged for 24 hours to the obtained transparent solution, stir mechanically for 0.5 hours, and then add dropwise 15.79g of orthosilicon Ethyl acetate, so that the SiO of two silicon sources (treated water glass and tetraethyl orthosilicate) 2 The molar ratio is 0.13:1, and mechanically stirred for 2 hours to obtain the initial gel of mordenite, wherein the material molar ratio is: 35SiO 2 : 1Al 2 o 3 : 10Na 2 O: 750H 2 O. After aging for 24 hours, it was transferred to a polytetrafluoroethylene-lined autoclav...

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Abstract

The invention relates to an efficient two-silicon-source amine-free synthesis method for morphology-controllable large-size mordenite. The method comprises specific steps as follows: two kinds of different silicon sources are added sequentially, and large-size mordenite with different morphology is obtained through hydro-thermal synthesis. According to the synthesis method, tetraethoxysilane and pretreated sodium silicate are used as the silicon sources, no organic amine, inorganic ammonia or toxic fluoride is required in the synthesis method, the synthesis process is environment-friendly, the operation process is convenient, the synthesis time is short, and synthesized molecular sieve crystalline grains have the uniform size.

Description

technical field [0001] The invention relates to the field of synthesis of zeolite molecular sieves, in particular to a high-efficiency method for synthesizing a large-size mordenite with controllable morphology using dual silicon sources without amines. Background technique [0002] Zeolite molecular sieve is a microporous crystalline aluminosilicate material, which is used as an important catalyst in modern industry due to its strong acidity, high stability, excellent shape selectivity and reproducibility. Mordenite (MOR structure) is one of the earliest zeolites recognized by humans. It belongs to the orthorhombic crystal system and the space group is C. m C m ,Cell parameters Mordenite has a two-dimensional channel structure, in which the main channel is 12-membered ring channel; the other side-grown channel is a twisted pocket-shaped hole with a size of about Because the pore size on its side is too small, most reactant molecules cannot pass through, so MOR zeol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/26
Inventor 茹淼焱王蕊童伟益宋艳朵张琪
Owner SHANDONG UNIV
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