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Lamellar mordenite preparation method

A mordenite and lamella technology is applied in the field of preparation of lamellar mordenite, which can solve the problems of side reactions, shorten the life of molecular sieve, increase diffusion resistance and the like, and achieve the effect of a simple synthesis method.

Active Publication Date: 2017-03-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the micropore diameter (<1nm) of mordenite molecular sieves restricts the entry of reactant molecules with larger kinetic diameters into the pores of the molecular sieve on the one hand, and on the other hand increases the diffusion resistance of reactant molecules in the pores, resulting in side effects. The occurrence of reaction and carbon deposition seriously shorten the life of molecular sieves

Method used

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  • Lamellar mordenite preparation method

Examples

Experimental program
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Effect test

example 1

[0035] (1) Preparation of structure directing agent

[0036]Add 30g (0.35mol) of N-methyltetrahydropyrrolidine into the three-necked flask, dropwise add 33g (0.18mol) of 1,2-dibromoethane, slowly rise to reflux, the solution is white and slightly turbid, reflux for 12h and then cool down. Water and ethyl acetate were added for extraction, the oil phase and the water phase were separated, and then the water phase was distilled and dehydrated under reduced pressure to obtain 52.5 g of a yellow oil, which was 1,2-bis(N-methylpyrrolidine)ethane bromide. That 1 H-NMR spectrum chemical shift (300MHz, internal standard TMS, solvent CDCl 3 ) δ (ppm) is: 2.11 (8H, m), 2.92 (6H, s), 3.09 (8H, m), 3.65 (4H, s).

[0037] (2) Preparation of lamellar mordenite

[0038] Take 0.134g of sodium metaaluminate and add it to a 45mL polytetrafluoroethylene (Teflon) container, add 23.28g of deionized water, 0.7947g of sodium hydroxide, and 1.74g of 1,2-bis(N-methylpyrrolidine) ethyl Alkyl bromid...

example 2

[0043] Take 0.134g of sodium metaaluminate and add it to a 45mL Teflon container, add 11.64g of deionized water, 0.56g of sodium hydroxide, and 1.16g of 1,2-bis(N-methylpyrrolidine)ethane bromide as structure-guided Agent R, stirred for 30 minutes until uniform, then added 2g of white carbon black, mixed thoroughly for 15 minutes, and the molar ratio of each component was: SiO 2 / Al 2 o 3 =40,Na 2 O / SiO 2 =0.56,H 2 O / SiO 2 =20, R / SiO 2 = 0.10.

[0044] Put the above mixture into a 45mL steel autoclave with Teflon lining and seal it, place the autoclave in a rotary convection oven at 120°C, set the rotation speed at 20rpm, react for 2 days, and raise the temperature to 175°C °C, react for 6 days. Take out the autoclave and let it cool down rapidly to room temperature, separate the mixture on a high-speed centrifuge at 5000rpm, collect the solid, wash with deionized water until the washing liquid is free of bromide ions, and dry at 100°C for 5 hours to obtain sheet-layer...

example 3

[0046] Prepare the structure-directing agent by the method of example 1 (1) step, the difference is to replace 1,2-dibromoethane with 0.18mol of 1,4-dibromobutane to obtain 1,4-bis(N-methyl Pyrrolidine) butane bromide salt.

[0047] Take 0.134g of sodium metaaluminate and add it to a 45mL Teflon container, add 11.64g of deionized water, 0.56g of sodium hydroxide, and 1.25g of 1,4-bis(N-methylpyrrolidine)butane bromide respectively as the structure Directing agent R, stir for 30 minutes until uniform, then add 2g of white carbon black, mix thoroughly for 15 minutes, and the molar ratio of each component is: SiO 2 / Al 2 o 3 =40,Na 2 O / SiO 2 =0.56,H 2 O / SiO 2 =20, R / SiO 2 = 0.10.

[0048] Put the above mixture into a 45mL steel autoclave with Teflon lining and seal it, place the autoclave in a rotary convection oven at 120°C, set the rotation speed at 20rpm, react for 2 days, and raise the temperature to 175°C °C, react for 6 days. Take out the autoclave and let it cool...

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Abstract

The invention relates to a lamellar mordenite preparation method, which comprises: (1) dissolving an inorganic alkali, an aluminum source and a structure-directing agent (R) in water and uniformly mixing to prepare a solution, wherein the structure-directing agent is a 1,n-bis(N-methylpyrrolidine)alkylene bromine salt having the structure formula represented by a formula (I), and n is 2-5; (2) adding a silicon source to the solution prepared in the step (1), and uniformly mixing to prepare a colloid or solid-liquid mixture, wherein the molar ratios of the added reactants comprise that the SiO2 / Al2O3 is 10-50, the H2O / SiO2 is 5-50, the R / SiO2 is 0.05-0.5, and the M2O / SiO2 is 0.05-1.0, and the M2O is an alkali metal oxide; and (3) carrying out hydrothermal crystallization for 1-5 days at a temperature of 80-140 DEG C under autogenous pressure, heating to a temperature of 150-250 DEG C, carrying out hydrothermal crystallization for 6-14 days under autogenous pressure, collecting the solid product after the crystallization, washing, and drying, wherein the obtained product has characteristics of high crystallinity, small grain thickness, and simple synthesis method. The formula (I) is defined in the specification.

Description

technical field [0001] The invention is a preparation method of mordenite, specifically, a preparation method of lamellar mordenite. Background technique [0002] Mordenite was first synthesized by Barrer in the 1940s. It has a one-dimensional twelve-membered ring straight cylindrical channel (pore diameter is 0.695nm × 0.581nm), in toluene disproportionation, alkylation, C 8 It exhibits excellent catalytic performance in the isomerization of aromatics and the selective disproportionation of toluene. However, the micropore diameter (<1nm) of mordenite molecular sieves restricts the entry of reactant molecules with larger kinetic diameters into the pores of the molecular sieve on the one hand, and on the other hand increases the diffusion resistance of reactant molecules in the pores, resulting in side effects. The occurrence of reaction and carbon deposition will seriously shorten the life of molecular sieve. Therefore, the preparation of nano molecular sieves, hierarc...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 祝进成王永睿慕旭宏陈俊文刘松霖舒兴田杨吉春刘长令
Owner CHINA PETROLEUM & CHEM CORP
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