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Method for synthesizing molecular sieve containing transition metal heteroatom LTL structure

A technology of transition metals and heteroatoms, applied in the field of synthesizing LTL structural molecular sieves containing transition metal heteroatoms, can solve the problems of high preparation cost and technical requirements, complicated steps, poor catalytic performance, etc., and achieve wide and cheap raw material sources and simple process , to solve the effect of precipitation

Active Publication Date: 2014-07-23
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Li et al. (J.Phys.Chem.C 2011, 115, 3663) synthesized Sn-Beta and Xu et al. (J.Catal. 2011, 281, 263) synthesized Ti-MOR. The steps of this method are complicated, and the preparation cost and technical requirements High, and the hydrothermal stability of the product is poor, the active site is easy to lose, and the catalytic performance is poor, which is still limited to the preparation and application in the laboratory

Method used

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  • Method for synthesizing molecular sieve containing transition metal heteroatom LTL structure
  • Method for synthesizing molecular sieve containing transition metal heteroatom LTL structure
  • Method for synthesizing molecular sieve containing transition metal heteroatom LTL structure

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Experimental program
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Effect test

Embodiment 1

[0023] Dissolve 1.76 g of cobalt nitrate hexahydrate (metal source) in 19 mL of deionized water, add 2.30 g of triethanolamine (coordination complexing agent) and stir to form a mixture; 2.73 g of aluminum hydroxide (aluminum source) and 9.35 g of hydrogen Dissolve potassium oxide in 10 mL of deionized water and stir to form a mixed solution; then mix the above two mixed solutions and add 40.05 g of silica sol solution, stir well and then conduct hydrothermal crystallization reaction at 170 °C for 36 hours, and the reaction solution is filtered and washed After drying at 200 °C, the Co-LTL molecular sieve with transition metal heteroatom-containing LTL structure was obtained.

Embodiment 2

[0025] Dissolve 0.62 g manganese acetate tetrahydrate (metal source) in 15.00 g deionized water, add 0.37 g tartaric acid (coordination complexing agent) and 1.92 g triethanolamine (coordination complexing agent) (coordination complexing agent) and stir For a mixed solution; dissolve 1.57 g of pseudoboehmite (aluminum source) and 14.03 g of potassium hydroxide in 46.50 g of deionized water and stir to form a mixed solution; then mix the above two mixed solutions and add 40.05 g of silica sol solution, stir After uniformity, the hydrothermal crystallization reaction was carried out at 170 °C for 36 hours. The reaction solution was filtered, washed and then dried at 200 °C to obtain a Mn-LTL molecular sieve with a transition metal heteroatom-containing LTL structure.

Embodiment 3

[0027] Dissolve 3.15 g nickel sulfate hexahydrate (metal source) in 71.42 g deionized water, then add 11.14 g triethanolamine hydrochloride (coordination complexing agent), 1.88 g pseudoboehmite (aluminum source), 16.36 g Potassium hydroxide and 12.02 g of white carbon black (fuming silica gel), stirred evenly, crystallized at 160 °C for 50 hours, the reaction solution was filtered and washed, and then dried at 200 °C to obtain a product with transition metal heteroatoms Ni-LTL molecular sieve with LTL structure.

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Abstract

The invention discloses a method for synthesizing a molecular sieve containing a transition metal heteroatom LTL structure. The method is characterized by comprising the following steps: mixing a heteroatom metal source, a coordinating complexing agent, an aluminum source, potassium hydroxide, a silicon source and water according to the atomic molar ratio of (0.001-0.1): (0.1-1.0): (0.04-0.2): (0.7-1.2): 1.0: (12-50), uniformly stirring, then performing crystallization reaction at the temperature of 150-180 DEG C for 24-72h, performing suction filtration and washing on a reaction solution, and then drying at the temperature of 100-200 DEG C to prepare a product, namely the molecular sieve containing the transition metal heteroatom LTL structure. Compared with the prior art, the method has the advantages of simple process, a variety of applicable heteroatom metals, extensive raw material sources and low cost, and can better solve the difficult problem of precipitation of a heteroatom transition metal source under strong alkaline conditions, thereby being a preparation process for synthesizing the molecular sieve containing the transition metal heteroatom LTL structure, which is easy to realize industrial implementation, mild in reaction conditions and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of inorganic chemical synthesis, in particular to a method for synthesizing a transition metal heteroatom-containing LTL structure molecular sieve. Background technique [0002] Microporous molecular sieves have uniform pore structure, suitable acidity and good hydrothermal stability, and have been widely used in petrochemical and fine chemical industries. L molecular sieves (LTL structure) with 7.1×7.1? one-dimensional twelve-membered ring straight channels are mainly used in chemical processes and adsorption such as catalytic reforming, aromatization, catalytic cracking and dehydrocyclization. Traditional molecular sieves are mainly used in chemical processes such as acid catalysis. Introducing transition metal ions into the molecular sieve framework and synthesizing heteroatom molecular sieves can make the molecular sieve have catalytic oxidation performance, thereby expanding the catalytic application o...

Claims

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Application Information

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IPC IPC(8): C01B39/32B01J29/63B01J29/64
Inventor 吴鹏薛凯吴海虹
Owner EAST CHINA NORMAL UNIVERSITY
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