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Preparation method of efficient acid-resistant mordenite molecular sieve

A mordenite and acid-resistant technology, applied in the field of inorganic molecular sieve technology synthesis, can solve the problems of long synthesis time, low efficiency, unknown long-term strong acid resistance, environmental pollution, etc. The effect of uniform distribution of aluminum elements

Pending Publication Date: 2022-01-28
CHANGZHOU UNIV
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Problems solved by technology

[0004] Aiming at the problems that the above synthetic mordenite uses organic templates to pollute the environment, the synthesis time is long and the efficiency is low, and the long-term strong acid resistance is unknown, the present invention provides a method for preparing a high-efficiency acid-resistant mordenite molecular sieve. source and seed crystal, which greatly shortens the time required, and the prepared mordenite has long-term acid resistance, and makes its crystallization strength increase in a very short synthesis time

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  • Preparation method of efficient acid-resistant mordenite molecular sieve
  • Preparation method of efficient acid-resistant mordenite molecular sieve
  • Preparation method of efficient acid-resistant mordenite molecular sieve

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Embodiment 1

[0037]The ratio of the synthetic solution is 8Na 2 O:36SiO 2 :1.4Al 2 o 3 :1600H 2 O:8.2NaF. The specific operation is: divide the deionized water into three parts, add sodium hydroxide to one part of deionized water to dissolve, add silica sol to the sodium hydroxide solution to form a silicon source precursor solution; add sodium metaaluminate to another part Dissolve in a portion of water to form an aluminum source precursor solution; add the aluminum source precursor solution drop by drop to the silicon source precursor solution under stirring, and stir at room temperature for 1 hour; dissolve sodium fluoride in the last portion of deionized water, and add it to the aforementioned The solution was stirred at room temperature for 1h. Then add the seed crystal and control the mass concentration of the seed crystal to 0.7wt%, transfer it to the reaction kettle after stirring for 30min, and synthesize at 180°C for 12h, and the crystallized product is centrifuged repeatedl...

Embodiment 2

[0039] Synthetic proportioning is constant, and the hydrothermal synthesis time is changed into 18h, and all the other synthetic conditions are identical with embodiment 1, and solid product is pure mordenite through XRD analysis ( figure 1 b), SEM characterization results are micron-scale grains, the shape is flat, and the grain size is about 2-3 microns ( Figure 5 c), analyzed by EDS ( Figure 10 ), the distribution of Al elements is uniform. Gained mordenite is acid-treated, and the treatment conditions are exactly the same as Example 1, and the acid-treated product is characterized by XRD ( figure 2 b) with no acid treatment ( figure 1 b) In comparison, the crystallization strength has only decreased by 4%, and the SEM characterization results show that the surface morphology remains good ( Figure 5 d).

Embodiment 3

[0041] Change the ratio of synthetic liquid to 9.5Na 2 O:39SiO 2 :1.7Al 2 o 3 :1700H 2 0:14NaF, all the other synthesis conditions are identical with embodiment 1, and solid product is pure mordenite ( figure 1 c), SEM characterization results are micron-scale grains, the shape is oval, and the grain size is about 2-3 microns ( Figure 5 e), analyzed by EDS ( Figure 11 ), the distribution of Al elements is uniform. Gained mordenite is acid-treated, and the treatment conditions are exactly the same as Example 1, and the acid-treated product is characterized by XRD ( figure 2 c) with no acid treatment ( figure 1 c) In comparison, the crystallization strength has only decreased by 4%, and the SEM characterization results show that the surface morphology remains good ( Figure 5 f).

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Abstract

The invention belongs to the technical field of synthesis of inorganic molecular sieves, provides a preparation method of an efficient acid-resistant mordenite molecular sieve, and mainly aims to solve the problems of overlong crystallization time and low efficiency during synthesis of mordenite. The method is mainly characterized in that a mordenite molecular sieve is taken as a seed crystal, sodium fluoride is taken as a mineralizing agent, and is added into a template-free synthetic mother solution, so that spatial distribution of an aluminum element in the mordenite is optimized, the mordenite with excellent crystallinity and higher acid resistance is induced and synthesized by a kettle pressure hydrothermal crystallization method, the synthesis time is shortened from 48 hours to 12 hours, and after the mordenite prepared by the method is subjected to acid treatment for 12 days in a 1 mol / l HCl solution, the crystallinity is still high, the surface appearance is basically unchanged, and the acid resistance is strong.

Description

technical field [0001] The invention belongs to the technical synthesis field of inorganic molecular sieves, and relates to a preparation method of high-efficiency acid-resistant mordenite molecular sieves. Background technique [0002] Mordenite (MOR) is an important class of microporous molecular sieves in industry. It has a uniform pore structure, suitable acid resistance and good hydrothermal stability, and has parallel elliptical twelve-membered rings (0.65 ×0.70nm) and eight-membered ring (0.26×0.57nm) straight channel, and the two parallel channels are connected through the eight-membered ring channel (0.34×0.48nm) in the b-axis direction. As a catalytic material, mordenite is widely used in the field of petrochemical industry. It shows excellent catalytic performance in the reaction processes of dimethyl ether carbonylation, alkylation, hydrocracking and so on. Due to its good acid resistance and hydrothermal stability, it has passed The preparation of mordenite mem...

Claims

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Application Information

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IPC IPC(8): C01B39/26
CPCC01B39/26C01P2002/72C01P2004/03C01P2004/61
Inventor 任秀秀杨胜杰钟璟徐荣左士祥
Owner CHANGZHOU UNIV
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