Method for synthesizing zeolite ZSM-48

A technology of ZSM-48 and zeolite, applied in the field of hydrothermal synthesis of ZSM-48 zeolite

Inactive Publication Date: 2011-05-04
SHANXI DATONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] U.S. Patent 4,423,021 first discloses the synthetic method of ZSM-48 zeolite, and this method is to use the organic diamine compound that contains 4~12 carbon atoms as structure directing agent, is about the oxide source of silicon, alkali metal source, water and structure The directing agent is composed of a mixture in a certain proportion, reacted at 160°C for 2 to 3 days, and the product ZSM-48 zeolite crystal is obtained by cooling, filtering, and washing with water, but the ZSM-48 zeolite synthesized by this method contains almost no aluminum, so almost not acidic

Method used

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  • Method for synthesizing zeolite ZSM-48
  • Method for synthesizing zeolite ZSM-48

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0025] I, structure directing agent N, the preparation of N-diethylhexamethyleneimine quaternary ammonium base

[0026] Into a 250 ml three-necked flask equipped with a stirrer, a reflux condenser and a dropping funnel, 39.6 g (0.4 mol) of hexamethyleneimine (hexamethyleneimine) and 60 ml of water were added. Heating with a water bath kept the reaction mixture at about 35° C., and added 21.8 g (0.2 mol) of bromoethane dropwise under stirring. After the addition, the stirring was continued for 8 hours at about 35°C. After cooling, the upper organic phase was separated, dried overnight with solid potassium hydroxide, and then distilled to collect fractions at 147-149° C. to obtain 20.3 g (0.16 moles) of N-ethylhexamethyleneimine. After confirming its chemical structure by NMR spectrum, IR spectrum and elemental analysis, 20.3g (0.16 mole) N-ethylhexamethyleneimine was dissolved in 60 milliliters of acetone, and excess bromoethane (26.2g 0.24 mole) was added , stirred at room t...

Embodiment approach 2

[0030] I, structure directing agent N, the preparation of N-diethylhexamethyleneimine quaternary ammonium base

[0031] Into a 250 ml three-necked flask equipped with a stirrer, a reflux condenser and a dropping funnel, 49.5 g (0.5 mol) of hexamethyleneimine (hexamethyleneimine) and 80 ml of water were added. Heating with a water bath kept the reaction mixture at about 30°C, and added 23.98 g (0.22 moles) of bromoethane dropwise under stirring. After the addition, the stirring was continued for 10 hours at about 30°C. After cooling, the upper organic phase was separated, dried overnight with solid potassium hydroxide, and then distilled to collect fractions at 147-149°C to obtain 22.8 g (0.18 moles) of N-ethylhexamethyleneimine. After confirming its chemical structure by NMR spectrum, IR spectrum and elemental analysis, 22.8g (0.18 moles) of N-ethylhexamethyleneimine was dissolved in 50 milliliters of acetone, and excess bromoethane (28.3g 0.26 moles) was added , stirred at ro...

Embodiment approach 3

[0035] I, structure directing agent N, the preparation of N-diethylhexamethyleneimine quaternary ammonium base

[0036] Into a 500 ml three-necked flask equipped with a stirrer, a reflux condenser and a dropping funnel, 99.0 g (1.0 mol) of hexamethyleneimine (hexamethyleneimine) and 200 ml of water were added. Heating with a water bath kept the reaction mixture at about 25°C, and added 49.1 g (0.45 mol) of bromoethane dropwise under stirring. After the addition was complete, stirring was continued for 16 hours at about 25°C. After cooling, the upper organic phase was separated, dried overnight with solid potassium hydroxide, and then distilled to collect fractions at 147-149°C to obtain 48.2 g (0.38 moles) of N-ethylhexamethyleneimine. After confirming its chemical structure by NMR spectrum, IR spectrum and elemental analysis, 48.2g (0.38 moles) of N-ethylhexamethyleneimine was dissolved in 120 milliliters of acetone, and excess bromoethane (54.5g 0.5 moles) was added , stir...

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Abstract

The invention provides a method for synthesizing zeolite ZSM-48, belonging to the technical field of inorganic chemistry and catalytic chemistry. The invention is characterized in that the method comprises the steps of mixing silicon source, aluminium source, alkali metal (M) source, structure guiding agent (R) N, N-dimethyl hexamethyleneimine quaternary ammonium base and water to prepare a reaction mixture with molar ratios that SiO2/Al2O3 is equal to 60-2000, H2O/SiO2 is equal to 10-100, OH<->/SiO2 is equal to 0.1-2.0, M/SiO2 is equal to 0.05-1.0 and R/SiO2 is equal to 0.05-1.0, carrying out hydrothermal crystallization on the reaction mixture at the temperature of 120-180 DEG C for 1-15 days, washing and drying products after crystallization is completed, thus obtaining the zeolite ZSM-48. By adopting the method provided by the invention, zeolite ZSM-48 with the ratio of silicate to aluminium being less than 150 can be synthesized.

Description

technical field [0001] A method for synthesizing ZSM-48 zeolite of the present invention belongs to the technical field of inorganic chemistry and catalytic chemistry, and specifically relates to a hydrothermal synthesis using N,N-diethylhexamethyleneimine quaternary ammonium base as a structure-directing agent Method for ZSM-48 zeolite. Background technique [0002] ZSM-48 is a kind of high-silica zeolite, which belongs to the orthorhombic crystal structure. It has 10-membered pore openings without interlaced linear channels. The channels are connected by 5-membered rings, and the diameter of the pores is about 0.6nm. The zeolite can be widely used in catalytic reactions of hydrocarbon conversion, such as aromatic hydrocarbon alkylation, isomerization, disproportionation, methanol conversion and the like. [0003] U.S. Patent 4,423,021 first discloses the synthetic method of ZSM-48 zeolite, and this method is to use the organic diamine compound that contains 4~12 carbon at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 晋春刘建红吕纯琴马宏芳郭永
Owner SHANXI DATONG UNIV
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