Preparation method and application of mordenite molecular sieve

A technology of mordenite and molecular sieve, which is applied in the direction of mercerized crystalline aluminum silicate zeolite, molecular sieve catalyst, molecular sieve and alkali exchange compound, etc., which can solve problems such as equipment corrosion, subsequent application of molecular sieve, and serious environmental pollution

Pending Publication Date: 2021-04-13
YANCHANG ZHONGKE (DALIAN) ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of sodium chloride / sodium sulfate as an additive in the synthesis process leads to serious equipment corrosion and environmental pollution, which has a certain impact on the subsequent application of molecular sieves

Method used

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  • Preparation method and application of mordenite molecular sieve
  • Preparation method and application of mordenite molecular sieve
  • Preparation method and application of mordenite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～8

[0079] Step 1: mix sodium hydroxide, aluminum source (the aluminum source used in embodiment 1 to embodiment 4 is sodium aluminate, the aluminum source used in embodiment 5 to embodiment 8 is aluminum sulfate) and water, add 30wt% silica sol and cetyltrimethylammonium bromide were stirred evenly, and then transferred to a stainless steel high-pressure hydrothermal reactor for pre-crystallization to obtain a silica-alumina precursor with a hydroxonite and mordenite structure.

[0080] Step 2: Mix sodium hydroxide, sodium aluminate / aluminum sulfate and water, then add 30 wt% silica sol and tetraethylammonium hydroxide, stir and age to obtain the structure-oriented sol.

[0081] Step 3: Mix the silicon-aluminum precursor obtained in step 1 and the structure-oriented sol obtained in step 2 in a certain proportion, stir evenly, and transfer the sol mixture to a stainless steel high-pressure hydrothermal reaction kettle for crystallization; after the crystallization is completed, the...

Embodiment 9

[0110] XRD analysis and characterization adopts X'Pert PRO X-ray diffractometer of PANalytical Company in the Netherlands, Cu target, Kα radiation source (λ=0.15418nm), voltage 40KV, current 40mA; SEM test instrument used is Hitachi SU8020 field emission Scanning electron microscope with an accelerating voltage of 2kV. The XRD pattern test was carried out on samples 1-8 and the intermediate product silicon-aluminum ratio precursor when preparing samples 1-8, with sample 7 as a typical representative, figure 1 It is the XRD spectrum of the silicon-aluminum precursor of sample 7. It can be seen that the sample has obvious structural characteristics of mordenite, but at the positions of 4.38°, 8.91°, 25.81° and 27.66°, hydroxosilicate zeolite appears at the same time Characteristic peaks of the structure (Kenyaite). image 3 It is the XRD spectrum of sample 7 of high silicon-aluminum ratio mordenite molecular sieve. It can be seen that this sample has obvious characteristic peak...

Embodiment 10

[0113] The product analysis was carried out on Fuli GC9790 gas chromatograph, HP-PLOT / Q column, FID detector; the conversion rate of dimethyl ether (DME) and the selectivity data of methyl acetate (MA) were calculated according to the area normalization method .

[0114] The mordenite molecular sieve catalyst samples prepared in the above examples and comparative examples were pressed into tablets, crushed and sieved, and 1g of 20-40 mesh catalyst was weighed and loaded into a fixed-bed reactor. 2 In-situ pretreatment for 3 hours, lower the temperature to 190°C, adjust the reaction pressure to 2.0MPa for activity evaluation, the reaction time is 12 hours, the feed volume ratio DME (dimethyl ether): N 2 : CO=1:45:4, the volume space velocity is 1600h -1 . Table 4 shows the catalyst evaluation results for the carbonylation of dimethyl ether to methyl acetate.

[0115] Table 4 Evaluation results of different dimethyl ether carbonylation catalyst samples

[0116] nam...

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Abstract

The invention discloses a preparation method of a mordenite molecular sieve with a high silica-alumina ratio. The preparation method comprises the following three steps: (1) carrying out pre-crystallization on a mixture I containing a silicon source I, an aluminum source I, hydroxide of the alkali metal ion M', a template agent R1 and water to obtain a silicon-aluminum precursor; (2) aging a mixture II containing a silicon source II, an aluminum source II, hydroxide of alkali metal ions M, a template agent R2 and water to obtain structure-oriented sol; and (3) mixing the silicon-aluminum precursor and the structure-oriented sol, carrying out hydrothermal crystallization, and roasting to obtain the mordenite molecular sieve. According to the method, the mordenite molecular sieve with the silica-alumina ratio higher than 40 can be prepared, the mordenite molecular sieve is used as a catalyst for synthesizing methyl acetate through dimethyl ether carbonylation, the conversion rate of dimethyl ether is high, and the stability of the catalyst is obviously superior to that of a dimethyl ether carbonylation catalyst prepared from the mordenite molecular sieve synthesized through a one-step method under the same conditions.

Description

technical field [0001] The application relates to a preparation method and application of a mordenite molecular sieve, belonging to the technical field of chemical catalysis. Background technique [0002] Mordenite molecular sieve is a crystalline microporous aluminosilicate with 12-membered ring and 8-membered ring channel structure, suitable acidity and good hydrothermal stability. It has become an important catalytic material for petroleum refining and petrochemical industry , has important industrial application value in the fields of catalytic cracking, alkylation, hydroisomerization and dimethyl ether carbonylation. Zeolites with MOR structure are generally classified as SiO 2 / Al 2 o 3 The molar ratio of 10-12 is divided into two types. According to most of the existing synthesis techniques, most of the SiO prepared without the use of templates 2 / Al 2 o 3 Low-silica mordenite with a molar ratio of 5-10 is equivalent to natural mordenite. High-silica mordenite ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/26B01J29/18C07C69/14C07C67/37
CPCC01B39/265B01J29/18C07C67/37C01P2002/72C01P2004/30C07C69/14
Inventor 夏春晖裴仁彦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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