Method for promoting synthesis of ZSM-11 molecular sieve

A ZSM-11, molecular sieve technology, applied in the field of catalytic chemistry, to achieve the effects of high crystallinity, short crystallization time and large specific surface area

Active Publication Date: 2020-02-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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The rapid preparation of ZSM-11 molecular sieves by...

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  • Method for promoting synthesis of ZSM-11 molecular sieve
  • Method for promoting synthesis of ZSM-11 molecular sieve

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Experimental program
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Embodiment 1

[0033] Under stirring conditions, 9.83g silica sol (30.57wt.% SiO 2 , 0.327wt.% Na 2 O, 0.033wt.%Al 2 o 3 , 6 9.01wt.%H 2 O), 0.54g aluminum sulfate (≥99wt.%), 0.58g sodium hydroxide (96.0wt.%NaOH), 3.22g tetrabutylammonium bromide (TBABr, purity≥99wt.%), 7.51g N-methyl Base-2-pyrrolidone (NMP, ≥99wt.%) and 28.90 g of deionized water were added to the reaction kettle in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =60,Na 2 O / SiO 2 = 0.15, TBA + / SiO 2 =0.2,H 2 O / SiO 2 =40, NMP / SiO 2 = 1.5. Stir for 10 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (40 rpm) at 130°C for 0-90h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 120°C to obtain molecular sieve powder. figure 1 (a) is the change curve of the crystallinity of the crystallized product with the crystallization time....

Embodiment 2

[0037] In embodiment 1, silica sol is changed into white carbon black, aluminum sulfate is changed into aluminum powder, sodium hydroxide is changed into potassium hydroxide (≥99wt.%), tetrabutylammonium bromide is changed into tetrabutyl chloride Aqueous ammonium solution (purity ≥ 35wt.%) is added to the reactor in the same order under stirring conditions, and the molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =100,K 2 O / SiO 2 = 0.2, TBA + / SiO 2 =0.4, NMP / SiO 2 = 2.0, H 2 O / SiO 2 =15. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (30 rpm) at 150°C for 25h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 120°C to obtain molecular sieve powder. The XRD spectrum pattern of gained ZSM-11 product and figure 2 Similarly, the particle size is about 0.6um.

Embodiment 3

[0039] In embodiment 1, silica sol is changed into orthosilicate ethyl ester (≥99wt.%), aluminum sulfate is changed into aluminum chloride (≥99wt.%), tetrabutylammonium bromide is changed into tetrabutylammonium hydroxide, N-methyl-2-pyrrolidone is changed to N-ethyl-2-pyrrolidone (NEP, ≥99wt.%), and under stirring conditions, it is added to the reactor in the same order, and the molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =80,Na 2 O / SiO 2 = 0.4, TBA + / SiO 2 =0.1, NEP / SiO 2 = 1.0, H 2 O / SiO 2 =30. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (20 rpm) at 170°C for 18h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 120°C to obtain molecular sieve powder. The XRD spectrum pattern of gained ZSM-11 product and figure 2 Similarly, the particle size is about 0.7um.

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Abstract

The invention provides a method for promoting the synthesis of a ZSM-11 molecular sieve. The method comprises the steps that a silicon source, an aluminum source, an inorganic base, a microporous templating agent and a crystal growth promoter R are sufficiently mixed, and obtained gel is subjected to short-time hydrothermal crystallization to rapidly prepare the ZSM-11 molecular sieve. The synthesis process is rapid, specifically, crystallizing is directly carried out at a suitable temperature for 10-90 hours, and the used crystal growth promoter is 2-pyrrolidone, N-methyl-2-pyrrolidone, N-ethyl-2-pyrrolidone, N-isopropyl-2-pyrrolidone or a mixture thereof. The ZSM-11 molecular sieve with high crystallinity, pure crystal phase, controllable particle size and wide range is quickly preparedby using the low-cost crystal growth promoter and through a one-step method, the method is instead of a traditional method to quickly obtain the ZSM-11 molecular sieve, and the method is an economicaland fast method to obtain the ZSM-11 molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and in particular relates to a method for promoting the synthesis of ZSM-11 molecular sieves. Background technique [0002] ZSM-11 is a molecular sieve first developed by Mobil Corporation in the early 1970s (USP3,709,979), belonging to Pentasil type zeolite, tetragonal crystal system, and its unit cell parameter is: a=20.270 b=20.270 c=13.459 α=90.000°, β=90.000°, γ=90.000°, the skeleton density is 17.4T / 1000 The channels of ZSM-11 molecular sieve are formed by the intersection of two-dimensional straight channels (0.51nm*0.55nm) of elliptical ten-membered rings. [0003] Although ZSM-11 molecular sieve has many potential catalytic functions, its preparation process faces difficulties such as long preparation period, high cost, and easy generation of miscellaneous crystals. Therefore, researchers began to work on the rapid and precise synthesis of ZSM-11 molecular sieves. [Z...

Claims

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Application Information

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IPC IPC(8): C01B39/36
CPCC01B39/365C01P2002/72C01P2004/62
Inventor 刘盛林杨传禹赵东璞辛文杰徐龙伢朱向学
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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