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Preparation method of ZSM-48 molecular sieve

A molecular sieve and organic base technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem that the pure phase ZSM-48 molecular sieve cannot be synthesized, and achieve the effect of good catalytic performance and high crystallinity

Active Publication Date: 2017-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Subsequent research found that tetramethylammonium ion was used as template and sodium hydroxide was used as alkali source, and no seed crystal or other template was added. The synthesized product was mainly ZSM-39 molecular sieve, and pure phase ZSM-48 molecular sieve could not be synthesized.

Method used

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  • Preparation method of ZSM-48 molecular sieve
  • Preparation method of ZSM-48 molecular sieve
  • Preparation method of ZSM-48 molecular sieve

Examples

Experimental program
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example 1

[0034] Add 7.5 g (0.047 mol) of bis(dimethylaminoethyl) ether and 100 mL of isopropanol into a two-necked flask, and stir evenly. At 25°C, 11.4g (0.047mol) of 1,6-dibromohexane was slowly added dropwise, heated to reflux temperature for 30min, the solution changed from colorless to white turbidity, and then reacted at reflux temperature for 12h, cooled to 25 ℃, 150 mL of ethyl acetate was added and stirred for 15 min. Filtration, the obtained solid was washed with ethyl acetate to give 13.1 g of white solid as 4,4,11,11-tetramethyl-1-oxo-4,11-diazacyclotridecane-4,11-di Bromide salt, i.e. the compound in which n is 4 in formula (I), its melting point is 230°C, 1 H-NMR spectrum chemical shift (300MHz, internal standard TMS, solvent D 2 O) is: 1.36(4H,t), 1.17(4H,t), 3.06(12H,s), 3.33(4H,t), 3.56(4H,t), 3.93(4H,t).

example 2

[0036] The diazoxane dibromide salt was prepared as in Example 1, except that 12.06 g (0.047 mol) of 1,8-dibromooctane was used instead of 1,6-dibromohexane to give 4,4, 13,13-tetramethyl-1-oxo-4,13-diazacyclopentadecane-4,13-dibromo salt 14.08g, i.e. the compound of formula (I) where n is 6, its melting point is 230.3°C, 1 H-NMR spectrum chemical shift (300MHz, internal standard TMS, solvent CDCl 3 )δ(ppm): 1.36(t, 4H), 1.73(s, 4H), 3.05(s, 12H), 3.33(t, 4H), 3.56(t, 4H), 3.92(t, 4H).

example 3

[0038] Take 0.134g of sodium metaaluminate and add it to a 45mL polytetrafluoroethylene (Teflon) container, add 14.45g of deionized water, 13.69g of tetraethylammonium hydroxide solution with a concentration of 35% by mass, 1.976g of 4,4, 11,11-Tetramethyl-1-oxo-4,11-diazacyclotridecane-4,11-dibromo salt was used as structure directing agent (R), stirred for 30 minutes until uniform, and then added 2g white carbon black , stir for 5 minutes and mix thoroughly, wherein the molar ratio of each component is: SiO 2 / Al 2 O 3 =40, TEAOH / SiO 2 =1.0, H 2 O / SiO 2 =40, R / SiO 2 =0.15, Na 2 O / SiO 2 = 0.12.

[0039] The above mixture was put into a 45 mL steel autoclave with Teflon lining, capped and sealed, and the autoclave was placed in a rotating convection oven with a rotating speed of 20 rpm, reacted at 120° C. for 4 days, and then heated to 160 °C. °C for 10 days. Take out the autoclave and make it rapidly cooled to room temperature, separate the mixture on a high-speed c...

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Abstract

The invention discloses a preparation method of a ZSM-48 molecular sieve. The preparation method comprises dissolving an organic base, an aluminum source and a structure-directing agent (R) shown in the formula (I) in water, mixing uniformly the materials, wherein in the formula (I), n represents 4 to 7, adding a silicon source into the mixed solution, carrying out uniform mixing, wherein in the reactants, a molar ratio of SiO2 / Al2O3 is 10 to 50, a molar ratio of BA / SiO2 is 0.1 to 2.0, a molar ratio of H2O / SiO2 is 5 to 50, a molar ratio of R / SiO2 is 0.05 to 0.5, a molar ratio of M2O / SiO2 is 0.05 to 0.3, M2O represents an alkali metal oxide and BA represents an organic base, carrying out hydrothermal crystallization on the reactants at a temperature of 80-140 DEG C for 1-5 days, heating the product to a temperature of 150-250 DEG C, carrying out hydrothermal crystallization for 5-14 days, collecting a solid product and drying the product. The molecular sieve contains nanoscale rod-like grains and has good catalytic performances.

Description

technical field [0001] The present invention is a preparation method of a silica-alumina molecular sieve, in particular, a preparation method of a molecular sieve with an MTW structure type. Background technique [0002] In the early 1980s, US4423021 first disclosed the use of C by Rollmann et al. 4 ~C 12 The method of synthesizing ZSM-48 molecular sieve with high silicon-aluminum ratio using organic diamine as structure-directing agent, but the product contains little or no aluminum, so the molecular sieve has almost no acidity. The structure type of ZSM-48 molecular sieve is MTW type, which belongs to the orthorhombic crystal structure. It has two-dimensional linear channels with 10-membered ring openings without passing through and staggered. The pores are connected by 5-membered rings. The ideal size is 0.55×0.56nm. ZSM-48 molecular sieve can be used as a catalyst for the conversion of methanol to gasoline (MTG) or synthesis gas (CO+H 2 ) catalysts for direct conversi...

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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