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Preparation method for immobilized Lewis acid

A technology of concentrated nitric acid and molecular sieves, which is applied in the preparation of carboxylic acid esters, organic compounds, sugar derivatives, etc., can solve the problems of high price, long production cycle, and inapplicability to large-scale preparation, and achieve wide applicability Effect

Inactive Publication Date: 2013-12-25
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method requires a long preparation cycle (up to 40 days)
Hermans et al. (Angew.Chem.Int.Ed.2012, 51:1–5) improved this method, using commercially available H-Beta as a raw material, and removing the internal Al with a nitric acid solution to form deAlBeta with a cavity , and then compare it with Sn(CH 3 COO) 2 Grinding and sintering in an air atmosphere can obtain tin-containing Beta molecular sieves, which saves the crystallization process and greatly shortens the preparation cycle. However, only limited volatile Sn(CH 3 COO) 2 Prepare Sn-Beta, and Sn(CH 3 COO) 2 High price, not suitable for large-scale preparation

Method used

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  • Preparation method for immobilized Lewis acid

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Embodiment 1

[0023] Synthesis of tin-containing molecular sieve (Sn-Beta): Mix 1 part of hydrogen-type β molecular sieve (H-β) with 20 parts of 13M nitric acid solution and heat to 100°C for 20 hours. Filtrate, wash with water until neutral, dry to remove water, and obtain dealuminated molecular sieve (deAlBeta). Then add to dissolve 10 parts by weight of anhydrous SnCl 4 In 100 parts of benzene, stirred at 25°C for 24h, filtered, washed with 1000mL benzene to remove free SnCl 4 , 550 ° C air activation 3h, after cooling to get Sn-Beta.

Embodiment 2

[0025] Synthesis of Ti-containing molecular sieve (Ti-Beta): Mix 1 part of hydrogen-type β molecular sieve (H-β) with 50 parts of 13M nitric acid solution and heat to 50°C for 48 hours. Filtrate, wash with water until neutral, dry to remove water, and obtain dealuminated molecular sieve (deAlBeta). Then add to dissolve 0.1 weight part of anhydrous TiCl 4 In 5 parts of chloroform, stirred at 10°C for 48h, filtered, washed with 500 parts of toluene to remove free TiCl 4 , Activated by air at 400°C for 20h, and obtained Ti-Beta after cooling.

Embodiment 3

[0027] Synthesis of In-containing molecular sieve (In-Beta): Mix 1 part of hydrogen-type β molecular sieve (H-β) with 50 parts of 8M nitric acid solution and heat to 150°C for 1 hour. Filtrate, wash with water until neutral, dry to remove water, and obtain dealuminated molecular sieve (deAlBeta). Then add to the solution with 10 parts by weight of anhydrous InCl 3 In 10 parts of methanol, stirred at 65°C for 48h, filtered, washed with 500 parts of chloroform to remove free InCl 3 , 800 ° C air activation 1h, after cooling In-Beta.

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Abstract

The invention discloses a preparation method for immobilized Lewis acid, belonging to the field of catalysis in organic synthesis. The immobilized Lewis acid referred to in the invention comprises Sn-Beta, Ti-Beta, In-Beta, Cu-Beta, Zn-Beta, Cr-Beta, etc. Solid acid with activity of Lewis acid is prepared by reacting a salt solution of a metal with a dealuminated molecular sieve and then carrying out sintering. The invention has the following advantages: raw materials are cheap and easily available, a generation period is short, the preparation method has high yield, the immobilized Lewis acid is easy to separate, reaction conditions are simple, and the immobilized Lewis acid can be extensively applied in the Baeyer-Villiger oxidation reaction, a reaction for preparation of methyl lactate from 1,3-dioxyacetone or a reaction for preparation of fructose from glucose.

Description

technical field [0001] The invention belongs to the field of catalysis in organic synthesis, in particular to a preparation method of immobilized Lewis acid. Background technique [0002] In recent years, with the continuous development of catalytic technology, it has become an important research content to immobilize the catalyst and realize the simple separation from the substrate. In traditional acid catalysts, The immobilization of acid is relatively mature, and the sulfonic acid group is mainly obtained by linking the sulfonic acid group with the supported matrix through the alkyl chain. However, this method cannot be used in the synthesis process of Lewis acid, so the research on the immobilization technology of Lewis acid is relatively backward. Corma, Davis et al. (Nature, 2001, 412: 424-425; PNAS, 2010, 107: 6164-6168) through tetraethyl orthosilicate, SnCl 4 ·H 2 After hydrolysis and crystallization of O etc., a tin-containing molecular sieve (Sn-Beta) is obta...

Claims

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Application Information

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IPC IPC(8): B01J29/70B01J29/76B01J29/78C07H3/02C07H1/00C07C69/68C07C67/00
Inventor 郭庆祥刘海峰邓理魏续瑞廖兵庞浩
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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