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Sol gel functionalized silicate catalyst and scavenger

A catalyst, silicate technology, applied in physical/chemical process catalysts, molecular sieve catalysts, catalyst activation/preparation, etc., can solve problems such as economic infeasibility, metal removal, product loss, etc.

Inactive Publication Date: 2008-04-23
QUEENS UNIV OF KINGSTON
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of these methods remove metals to the extent required by regulatory standards, they require additional reaction steps to be added to the process (see Garrett, 2004), or they result in significant loss of product, thus economically unfeasible

Method used

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  • Sol gel functionalized silicate catalyst and scavenger
  • Sol gel functionalized silicate catalyst and scavenger
  • Sol gel functionalized silicate catalyst and scavenger

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0205] Example 1. Preparation of coated SBA-15-SH material

[0206] To a suspension of SBA-15 suspended in anhydrous toluene (30 mL) or silica (1 g) was added dropwise (CH 3 O)Si(CH 2 ) 3 SH (1 mL, 5.3 mmol) and pyrimidine (1 mL, 12.3 mmol) (see Zhao et al., 1998 a and b). The reaction mixture was refluxed at 115°C for 24 hours. After cooling, the suspension was filtered and the solid residue was washed with methanol, ether, acetone and hexane to remove unreacted thiol. The washed solid was vacuum dried at room temperature to obtain a white powder. The Brauner Emmer Teller (BET) surface area (specific surface area) of SBA-15-SH is 410 m2 / g, and the sulfur content obtained through elemental analysis is 2.2 mmol / g, SiO 2 The BET surface area (specific surface area) of -SH is 297 m2 / g, and the sulfur content obtained by elemental analysis is 1.3 mmol / g.

Embodiment 2

[0207] Embodiment 2. Preparation of sol-gel SBA-15-SH material

[0208] Synthesis of SBA-15 material functionalized with 3-mercaptopropyltrimethoxysilane (MPTMS) versus pure silica form SBA-15 (see articles a and b published in 1998 by Zhao et al. ) is similar, only changes in the amount of mercaptopropyltrimethoxysilane (MPTMS), as can be seen in the article published in 2002 by Melero et al. Using a one-step method, tetraethyl orthosilicate (TEOS) was co-condensed with different proportions of mercaptopropyltrimethoxysilane (MPTMS) to synthesize samples, wherein the mercaptopropyltrimethoxysilane (MPTMS) was prepared in three Block copolymer polyethylene oxide 123 (P123, with EO 20 PO 70 EO 20 (Aldrich) premixed in the presence of the general chemical formula in which EO stands for ethylene oxide and PO stands for propylene oxide). Use 4 grams of P123, 120 milliliters of 2M hydrochloric acid, 30 milliliters of distilled water, with different ratios of orthoethyl silica...

Embodiment 3

[0209] The preparation of embodiment 3.SBA-15-SH Pd material

[0210] Under an inert gas atmosphere, place 50 mL of 0.05 M Pd(OAc) in a Schlenk flask 2 Soluble in anhydrous tetrahydrofuran (THF) solution. Add 1 gram of SBA-15-SH or SiO to the solution 2 -SH, the mixture was stirred at room temperature for 1 hour. Then the solid catalyst was obtained by filtration, washed with tetrahydrofuran, and then vacuum-dried at room temperature.

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PUM

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Abstract

This invention relates to materials suitable as metal scavengers and catalysts. The materials are prepared by functionalizing silicate materials such as silica or SBA-15 with a thiol or amine, or other functionalizing agent, in a sol gel process. In a preferred embodiment, the metal is palladium and the functionalizing agent is a thiol. The material may be used as a catalyst for the Suzuki-Miyaura and Mizoroki-Heck coupling reactions. The catalyst materials have extremely low metal leaching, are very stable, and are completely recyclable.

Description

[0001] related application [0002] This application claims priority from US Patent Application Serial No. 60 / 658,579, filed March 7, 2005, the entire contents of which are hereby incorporated by reference. technical field [0003] The present invention relates to a class of metal catalysts and scavengers for removing metals in aqueous and organic solutions. More particularly, the present invention relates to a class of metal catalysts based on functionalized solid phase supports, which are prepared by a sol-gel method. Background technique [0004] Metal-catalyzed reactions have become part of the standard approach to the synthesis of organic chemicals (see Diederich et al., 1998). For example, palladium catalysts are used to catalyze coupling reactions like the Mizoroki-Heck reaction and the Suzuki-Miyaura reaction, and provide a one-step method for constructing complex structures, such as those employed in pharmaceutical products. Metal-catalyzed reactions can also be u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/00B01J37/00B01D15/08C01B33/20
CPCB01J20/28083B01D15/00B01J20/32B01J20/3064B01J20/3204C01B33/12B01J20/28047B01J20/28011B01J20/3257C01B37/00B01J20/28007B01J20/10B01J20/3242B82Y30/00
Inventor 凯思琳·M·库顿穆特亚拉·萨特施亚历山德尔·布兰斯
Owner QUEENS UNIV OF KINGSTON
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