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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  • 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 ...

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

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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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