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A method for accelerating the synthesis of beta molecular sieves

A molecular sieve and uniform mixing technology, applied in the field of catalytic chemistry, can solve the problems of cumbersome preparation process, low product yield, low preparation reproducibility, etc., and achieve the effect of high crystallinity and simple preparation method

Active Publication Date: 2022-08-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To sum up, there are still some problems in the rapid synthesis method of Beta molecular sieve reported so far: such as complicated preparation process, low preparation reproducibility, low product yield, etc., which limit its industrial production to a certain extent.

Method used

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  • A method for accelerating the synthesis of beta molecular sieves
  • A method for accelerating the synthesis of beta molecular sieves

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under stirring conditions, 5.3 g of white carbon black (95.0 wt.% SiO 2 , 5.0wt.%H 2 O), 0.4g sodium aluminate (49.0wt.%Al 2 O 3 , 38.0wt.%Na 2 O, 13.0wt.%H 2 O), 0.13g sodium hydroxide (96.0wt.%NaOH), 22.4g tetraethylammonium hydroxide aqueous solution (TEAOH, purity ≥35wt.%), 3.64g butyrolactone (BL, ≥99wt.%), 9g Deionized water was added to the reactor in a certain order. The molar composition of the raw material mixture is: SiO2 / Al 2 O 3 =43.5, Na 2 O / SiO 2 =0.048, TEA + / SiO 2 =0.636, BL / SiO 2 =0.5, H 2 O / SiO 2 =16. Stir for 30min to make it fully mixed and evenly seal the synthesis kettle. Directly crystallize at 140°C for 0-72h. The reaction was quenched with tap water and centrifuged to give a solid product. Then wash with deionized water until neutral. Dry at 80°C overnight to obtain the original molecular sieve powder. figure 1 It is the change curve of the crystallinity of the crystallization product with the crystallization time. It can b...

Embodiment 2

[0041] Under stirring conditions, 19.5 g of water glass (26 wt. % SiO 2 , 8.2wt.%Na 2 O, 65.8wt.%H 2 O), 5.6g aluminum sulfate (≥99wt.%), 1.9g potassium hydroxide (≥99wt.%), 25g tetraethylammonium chloride aqueous solution (TEACl, purity≥35wt.%), 14.5g BL in a certain order into the reactor. The molar composition of the raw material mixture is: SiO 2 / Al 2 O 3 =10, K 2 O / SiO 2 =0.2, TEA + / SiO 2 =0.636, BL / SiO 2 =2.0, H 2 O / SiO 2 =16. Stir for 30min to make it fully mixed and evenly seal the synthesis kettle. Crystallize directly at 95°C for 90h. The reaction was quenched with tap water and centrifuged to give a solid product. Then wash with deionized water until neutral. Dry at 80°C overnight to obtain the original molecular sieve powder. The XRD pattern of the obtained Beta product is the same as figure 2 similar.

Embodiment 3

[0043] Under stirring conditions, 17.4g ethyl orthosilicate (≥99wt.%), 0.2g aluminum chloride (≥99wt.%), 2.7g sodium hydroxide, 3.5g tetraethylammonium hydroxide aqueous solution, 8.5g Valerolactone (VL, ≥99 wt.%) and 9 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 =200, Na 2 O / SiO 2 =0.4, TEA + / SiO 2 =0.1, VL / SiO 2 =1.0, H 2 O / SiO 2 =16. Stir for 30min to make it fully mixed and evenly seal the synthesis kettle. Crystallize directly at 120°C for 30h. The reaction was quenched with tap water and centrifuged to give a solid product. Then wash with deionized water until neutral. Dry at 80°C overnight to obtain the original molecular sieve powder. The XRD pattern of the obtained Beta product is the same as figure 2 similar.

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Abstract

The present invention provides a method for accelerating the synthesis of Beta molecular sieves. In the method, Beta molecular sieve is rapidly prepared by hydrothermal crystallization of gel obtained by fully mixing silicon source, aluminum source, inorganic base, microporous template agent and accelerator. The accelerators used are butyrolactone, valerolactone, caprolactone or mixtures thereof. The invention uses a cheap accelerator to rapidly obtain the Beta molecular sieve by one-step method, replaces the traditional seed crystal method to quickly obtain the Beta molecular sieve, and is an economical and fast method for obtaining the Beta molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of catalytic chemistry, and in particular relates to a method for accelerating the synthesis of Beta molecular sieves. Background technique [0002] Beta molecular sieve is a medium pore zeolite with a unique cage-free three-dimensional 12-membered ring large pore system, good catalytic stability, thermal stability and hydrothermal stability. A straight channel along the [100] and [010] orientations has a pore size of about 0.77×0.67nm; along the [001] direction is a curved channel running through the straight channel with a pore size of about 0.56×0.56nm. Beta molecular sieves have a wide range of industrial application values ​​and are mainly used in the catalytic conversion of hydrocarbons, such as: alkylation of benzene and olefins (production of ethylbenzene and cumene), transalkylation of heavy aromatics, hydrocarbon cracking, Hydroisomerization, etc. [0003] Although Beta molecular sieves have many...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B39/02B01J29/70
CPCC01B39/04C01B39/026B01J29/7007C01P2002/72Y02P20/52
Inventor 刘盛林王新怡楚卫锋赵东璞朱向学徐龙伢冯超辛文杰崔倩
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI