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Preparation method of hollow single crystal Beta molecular sieve

A molecular sieve and single crystal technology, applied in the field of catalytic chemistry, can solve the problems of cumbersome preparation process, harsh conditions and restrictions on industrial production of multi-stage porous or hollow Beta molecular sieves, and achieve high crystallinity, large specific surface area and pore volume, and simple The effect of the preparation method

Inactive Publication Date: 2018-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, the preparation process of the reported hierarchical porous or hollow Beta molecular sieves is cumbersome and the conditions are harsh, which limits its industrial production to a certain extent.

Method used

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  • Preparation method of hollow single crystal Beta molecular sieve
  • Preparation method of hollow single crystal Beta molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under stirring conditions, 5.3g of white carbon black (95.0wt.% SiO 2 , 5.0wt.%H 2 O), 0.4g sodium aluminate (49.0wt.%Al 2 o 3 , 38.0 wt.% Na 2 O, 13.0 wt.% H 2O), 0.13g sodium hydroxide (96.0wt.% NaOH), 22.3g tetraethylammonium hydroxide aqueous solution (TEAOH, purity ≥ 35wt.%), 25g N-methyl-2 pyrrolidone (NMP, ≥ 99wt.% ), 9g of deionized water were added to the reactor in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =43.5,Na 2 O / SiO 2 = 0.048, TEA + / SiO 2 =0.636, NMP / SiO 2 =3.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (30 rpm) at 140°C for 60h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.

[0037] figure 1 It is the powder X-ray diffraction pattern of the obtained molecular sieve powd...

Embodiment 2

[0042] Under stirring condition, 19.5g water glass (26wt.%SiO 2 , 8.2 wt.% Na 2 O, 65.8 wt.% H 2 O), 1.29g aluminum sulfate (≥99wt.%), 1.9g potassium hydroxide (≥99wt.%), 25g tetraethylammonium chloride aqueous solution (TEACl, purity ≥35wt.%), 25g N-methyl- 2 Pyrrolidone is added to the reaction kettle in a certain order. The molar composition of the raw material mixture is: SiO 2 / Al 2 o 3 =43.5, K 2 O / SiO 2 = 0.2, TEA + / SiO 2 =0.636, NMP / SiO 2 =3.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (100 rpm) at 100°C for 240h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.

[0043] The XRD spectrum pattern of gained Beta product and figure 1 Similarly, transmission electron microscopy (TEM) pictures show that it is a hollow single crystal structur...

Embodiment 3

[0045] Under stirring conditions, 17.4g ethyl orthosilicate (≥99wt.%), 2.0g aluminum chloride (≥99wt.%), 2.7g sodium hydroxide, 3.5g tetraethylammonium hydroxide aqueous solution, 43g N -Ethyl-2-pyrrolidone and 9g 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 =20,Na 2 O / SiO 2 = 0.4, TEA + / SiO 2 =0.1, NEP / SiO 2 =6.0,H 2 O / SiO 2 =16. Stir for 30 minutes to make it fully mixed and seal the synthesis kettle. Directly crystallize dynamically (80 rpm) at 100°C for 200h. The reaction was quenched with tap water and centrifuged to obtain a solid product. Then wash with deionized water until neutral. Dry overnight at 80°C to obtain molecular sieve powder.

[0046] The XRD spectrum pattern of gained Beta product and figure 1 Similarly, transmission electron microscopy (TEM) pictures show that it is a hollow single crystal structure with a particle size of about 312nm, N 2 Th...

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Abstract

The invention provides a preparation method of a hollow single crystal Beta molecular sieve. The method comprises the step that the hollow single crystal Beta molecular sieve is prepared by one-step hydrothermal crystallization of a gel formed by thoroughly mixing a silicon source, an aluminum source, an inorganic base, a microporous templating agent and an organic additive lactam R. A synthesizedproduct is formed by sequential stacking and connecting of primary nanoparticles, and the primary particle size is 10 to 30 nm; the preparation method of the hollow single crystal Beta molecular sieve takes inexpensive N-methyl-2-pyrrolidone or homolog thereof such as 2-pyrrolidone, N-ethyl-2-pyrrolidone, N-isopropyl-2-pyrrolidone as organic additives, the hollow single crystal Beta molecular sieve is synthesized by one-step method to replace a traditional two-step acid-base treatment method to obtain a hollow structure, the preparation method of the hollow single crystal Beta molecular sieveis an economical, efficient method for easily obtaining the hollow single crystal Beta molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry; in particular, it relates to a method for preparing a hollow single-crystal Beta molecular sieve. Background technique [0002] Beta molecular sieve is a medium-pore zeolite with a unique cage-free three-dimensional twelve-membered ring macropore system, good catalytic stability, thermal stability and hydrothermal stability. Along the [100] and [010] orientation linear channel, the pore diameter is about 0.77×0.67nm; along the [001] direction is a curved channel through the straight channel, the pore diameter is about 0.56×0.56nm. Beta molecular sieve has a wide range of industrial application value, mainly used in the catalytic conversion process of hydrocarbons, such as: alkylation of benzene and olefins (production of ethylbenzene, cumene), transalkylation of heavy aromatics, hydrocarbon cracking, Hydroisomerization, etc. [0003] Although Beta molecular sieve has many potential ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B82Y40/00
CPCB82Y40/00C01B39/04C01P2002/72C01P2004/03C01P2004/04C01P2006/12C01P2006/14C01P2004/50C01P2004/64C01B39/48
Inventor 徐龙伢赵东璞辛文杰刘盛林楚卫锋朱向学谢素娟陈福存
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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