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Preparation method of hydrogen type silica-alumina ZSM-48 molecular sieve

A technology of ZSM-48 and molecular sieve, which is applied in the field of preparation of silicon-aluminum molecular sieve, can solve the problems of high cost, limitation, high silicon-aluminum, etc., and achieve the effect of low cost

Active Publication Date: 2021-10-26
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In summary, although the synthesis of ZSM-48 molecular sieves with a silicon-aluminum ratio of less than 200 has made some progress, they often use templates with complex structures and high costs, which is not conducive to the large-scale use of ZSM-48 molecular sieves; Although ZSM-48 molecular sieves can also be synthesized by organic amines, the application of ZSM-48 molecular sieves as acidic catalysts is limited because of its high silicon-aluminum ratio (generally greater than 200).
In addition, although a ZSM-48 molecular sieve with a silicon-alumina ratio of less than 200 can be synthesized by using a template agent with a complex structure and high cost, due to the introduction of alkali metal during the synthesis process, the subsequent exchange process is necessary to obtain the hydrogen-form ZSM- 48 molecular sieve

Method used

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  • Preparation method of hydrogen type silica-alumina ZSM-48 molecular sieve
  • Preparation method of hydrogen type silica-alumina ZSM-48 molecular sieve
  • Preparation method of hydrogen type silica-alumina ZSM-48 molecular sieve

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preparation example Construction

[0020] More specifically, the preparation method provided by the invention comprises:

[0021] (1) Fully mix the silicon source and the template R to obtain the following molar composition as R / SiO 2 =0.01~0.50,H 2 O / SiO 2 =5~100 mixture, hydrothermal crystallization to obtain pure silicon ZSM-48 molecular sieve; wherein, the template R is selected from ethylenediamine, 1,3-propylenediamine, 1,4-butylenediamine, 1 , 5-pentanediamine, 1,6-hexanediamine, 1,7-heptanediamine, 1,8-octanediamine, 1,9-nonanediamine, one of the above-mentioned diamines with substituents or more mixtures, the relative crystallinity of the pure silicon ZSM-48 molecular sieve is ≥90%;

[0022] (2) Treat the mixture of organic base R1 and aluminum source in a closed reaction kettle at 50-190°C to obtain a tetracoordinated aluminum source; wherein, the organic base R1 is selected from tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, One or more of ammonium hydroxide, tetrapropylammonium hy...

Embodiment 1

[0042] With 400g silica sol (Shandong Yiming Industry and Trade Co., Ltd., 30%SiO 2 ), 48g 1,6-hexamethylenediamine (analytical grade, Sinopharm Chemical Reagent Co., Ltd.) and 260g water are fully mixed, and the reaction mixture has the following composition: R / SiO 2 =0.2,H 2 O / SiO 2 =15. The mixture was put into a crystallization tank and heated to 160°C for hydrothermal dynamic crystallization for 48 hours. After the crystallization is completed, it is filtered, washed, dried, and calcined at 580°C for 3 hours to obtain pure silicon ZSM-48 molecular sieve (96% crystallinity).

[0043] Weigh 1 gram of pseudo-boehmite (Changling Catalyst Factory, Al 2 o 3 Content 75%), it is mixed with 60g tetraethylammonium hydroxide aqueous solution (TEAOH content 20%), mixture molar ratio TEAOH / Al 2 o 3 =11. The mixture was placed in a polytetrafluoro-lined crystallization kettle, reacted at 150°C for 3 hours, and then cooled to room temperature to obtain a hydrothermal treatment p...

Embodiment 2

[0052] 281g ethyl orthosilicate (containing 28% SiO 2 , Beijing Chemical Reagent Company), 16.5g 1,6-hexamethylenediamine (analytical grade, Sinopharm Chemical Reagent Co., Ltd.) and 378g water are fully mixed, and the reaction mixture has the following composition (mol / mol, expressed in oxide form) : R / SiO 2 =0.1;H 2 O / SiO 2 =16. The mixture was put into a crystallization tank and heated to 160°C for hydrothermal dynamic crystallization for 48 hours. After the crystallization is completed, it is filtered, washed, dried, and calcined at 580°C for 3 hours to obtain a pure silicon ZSM-48 molecular sieve (98% crystallinity).

[0053] Weigh 1.12 grams of alumina (Changling Catalyst Factory, Al 2 o 3 content 98%), it is mixed with 54g tetrapropyl ammonium hydroxide aqueous solution (Beijing Jiayousheng New Technology Development Center, analytically pure, TPAOH content 25%), and the mixture mol ratio is TPAOH / Al 2 o 3=6.16, put it in a crystallization kettle with polytetraf...

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Abstract

The invention discloses a preparation method of a hydrogen type silicon-aluminum ZSM-48 molecular sieve. The preparation method is characterized in that a pure silicon ZSM-48 molecular sieve synthesized in a system without alkali metal or additional alkali metal is subjected to aluminum supplement treatment by an aluminum source, a product is recovered, and in the aluminum supplement process, the aluminum source is a tetra-coordinated aluminum source obtained by organic alkali dissolution treatment. The method for preparing the molecular sieve with the low silica-alumina ratio is low in cost, the prepared product does not need ammonium exchange, and the hydrogen type silica-alumina ZSM-48 molecular sieve is directly obtained after roasting.

Description

technical field [0001] The present invention relates to a preparation method of a silicon-aluminum molecular sieve, and further the present invention relates to a preparation method of a hydrogen-type silicon-aluminum ZSM-48 molecular sieve. Background technique [0002] The ZSM-48 molecular sieve with *MRE topology is a kind of high silica zeolite, which belongs to the orthorhombic crystal system. Its pore structure is one-dimensional linear channels with 10-membered ring openings, and the channels are connected by 5-membered rings. , the diameter of the orifice is 0.56nm×0.56nm. The 10-membered ring channel of ZSM-48 molecular sieve can be regarded as a six-membered ring ribbon composed of 20 T atoms. The channel moves 1 / 2 unit in the channel direction to form two kinds of connections between channels, one is curved Chain connection, one is 4-membered ring connection, and each tubular channel is adjacent to 4 tubular channels, so a variety of polymorphs can be formed betw...

Claims

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Application Information

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IPC IPC(8): C01B39/48B82Y30/00B82Y40/00
CPCC01B39/48B82Y30/00B82Y40/00C01P2002/72C01P2004/03C01P2004/34C01P2004/16C01P2004/64C01P2004/61
Inventor 王萍邢恩会方文秀毕云飞罗一斌
Owner CHINA PETROLEUM & CHEM CORP
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