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Preparation method and application of mordenite with high silica-alumina ratio

A technology of mordenite and high silicon-to-aluminum ratio, which is applied in the field of catalysis, can solve the problems of incomplete utilization of raw materials, emission of pollution, surplus of reaction materials, etc., and achieve the effects of improving the production of mordenite, avoiding pollution and reducing preparation costs.

Active Publication Date: 2021-03-23
YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

[0007] Aiming at the silicon-aluminum ratio of the molecular sieve hydrothermal synthesis product in the prior art is generally lower than the silicon-aluminum ratio of the raw material feeding, the raw material silicon-aluminum ratio (SiO 2 / Al 2 o 3 Molar ratio) is very high, the raw material can not be fully utilized and will increase the problem of cost. In addition, there are many reaction materials remaining in the filtrate after crystallization, and the emission pollution is serious

Method used

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  • Preparation method and application of mordenite with high silica-alumina ratio
  • Preparation method and application of mordenite with high silica-alumina ratio
  • Preparation method and application of mordenite with high silica-alumina ratio

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Experimental program
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Effect test

Embodiment 1～6

[0094] Step 1: Weigh a certain amount of sodium hydroxide, sodium aluminate, silica sol, cetyltrimethylammonium bromide and mix with water, stir evenly, and then transfer to a stainless steel high-pressure hydrothermal reaction kettle for pre-crystallization , to obtain a high silicon-aluminum ratio precursor solution with a hydroxonite structure. Step 2: mixing sodium hydroxide, sodium aluminate and water, then adding silica sol and tetraethylammonium hydroxide, stirring and aging to obtain a structure-oriented sol. Step 3: The silicon-aluminum precursor solution and the structure-oriented sol obtained in step 2 are mixed in a certain proportion, stirred evenly, and then transferred to a stainless steel high-pressure hydrothermal reaction kettle for crystallization; after the crystallization is completed, the product is press-filtered to obtain the filtrate after crystallization , the product was washed with deionized water until neutral, dried at 120°C for 12 hours, and calc...

Embodiment 7

[0096] Raw materials used, proportioning and test conditions are identical with step one, step two, step three and step four in embodiment 1. Wherein, the water in step two is completely replaced by the filtrate after crystallization obtained in step three in embodiment 1.

[0097] Among them, during the preparation of samples 1 to 7, the molar amount of raw materials, precrystallization temperature and time of the silica-alumina precursor with hydroxonite and mordenite are shown in Table 1 for details.

[0098] During the preparation of samples 1-7, the molar amounts of raw materials, crystallization temperature and time of the structure-oriented sol and comparative sample 1 are shown in Table 2 for details.

[0099] See Table 3 for the mass ratio of the silicon-aluminum precursor mixed with the structure-directed sol in samples 1 to 7 and the silicon-aluminum molar ratio of the mordenite sample obtained after the final test of comparative sample 1.

[0100] Table 1 Preparat...

Embodiment 8

[0137] Scanning electron microscope analysis (SEM) was performed on the high-silicon-aluminum-ratio mordenite samples prepared in the above examples. The instrument used in the SEM test was a Hitachi SU8020 field emission scanning electron microscope with an accelerating voltage of 2 kV.

[0138] Taking the sample 1 prepared in Example 1 as a typical example, figure 1 It is the SEM photo (500nm) of the silicon-aluminum precursor corresponding to sample 1, Figure 4 It is the SEM photograph (1 μm) of sample 1. Depend on figure 1 It can be seen that the sample has two zeolite structures of different sizes, of which the hydroxysilica zeolite is much larger in size. Depend on Figure 4 It can be seen that the finally obtained high-silicon-aluminum-ratio mordenite has a short columnar packing structure with a size of 30-60×200-500 nm.

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Abstract

The invention discloses a preparation method and application of mordenite with a high silica-alumina ratio. The preparation method of the mordenite with the high silica-alumina ratio comprises the following three steps: (1) carrying out pre-crystallization on an aluminum source, a silicon source, an alkali source, a template agent R1 and water under a certain condition to obtain a precursor with the high silica-alumina ratio; (2) stirring and aging the aluminum source, the silicon source, the alkali source, a template agent R2 and water (or a filtrate obtained after crystallization) accordingto a certain ratio at a certain temperature to prepare guide sol; and (3) mixing the precursor with the high silica-alumina ratio and the guide sol according to a certain ratio, and carrying out hydrothermal crystallization to obtain the mordenite with the high silica-alumina ratio. By using the method, the filtrate obtained after crystallization is effectively utilized, pollution is reduced, andthe mordenite with the silica-alumina ratio of 15-50 can be prepared; and the mordenite has excellent performance of synthesizing methyl acetate by carbonylation of dimethyl ether.

Description

technical field [0001] The application relates to a preparation method and application of a high-silicon-aluminum-ratio mordenite, which belongs to the technical field of catalysis. Background technique [0002] Mordenite is a crystalline microporous aluminosilicate with regular pore structure, suitable acidity and good hydrothermal stability. It is an important chemical catalytic material. It is used in catalytic cracking, alkylation, hydroisomerization It has important industrial application value in fields such as carbonylation of dimethyl ether and carbonylation of dimethyl ether. [0003] Mordenite is a better catalyst carrier for the carbonylation of dimethyl ether to methyl acetate, and its 12-membered and 8-membered ring channels provide suitable reaction conditions for the carbonylation of dimethyl ether. However, low-silicon-alumina mordenite is more prone to carbon deposition due to more acid sites, and high-silicon-alumina has longer service life and better stab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/26B01J29/18C07C67/37C07C69/14
CPCC01B39/265B01J29/18C07C67/37B01J2229/16C01P2002/72C01P2004/03C07C69/14
Inventor 裴仁彦夏春晖吕新新王国建刘骆安王建刘勇王辉
Owner YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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