Nano periodic mesoporous organic silicon oxide material and its synthetic method and its use

A technology of organic silicon oxide and synthesis method, which is applied in the direction of producing hydrocarbons from halogen-containing organic compounds, chemical instruments and methods, catalyst carriers, etc., can solve problems such as high cost, limited organic solubility, environmental pollution, etc., to prevent pollution Effect of reducing solubility limitation

Inactive Publication Date: 2007-04-11
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The Ullmann reactions reported so far are all carried out in organic solvents, using organometallic copper, nickel, and palladium as homogeneous catalysts. The use of heterogeneous catalysts generally requires the addition of phase transfer reagents such as crown ethers, PEG, etc., which inevitably brings environmental problems. to pollute
Water is the cleanest and safest solvent, but its ability to dissolve organic matter is limited, which is not conducive to organic synthesis. Obviously, the key to realize the clean Ullmann reaction in aqueous medium is to develop new and efficient catalysts
Although the homogeneous catalyst has high activity and excellent selectivity, its stability is poor, and it is difficult to separate from the product, resulting in high cost, and it is easy to cause heavy metal pollution during use.
Heterogeneous catalysts can overcome the above defects, but the activity and selectivity are generally not comparable to homogeneous catalysts

Method used

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  • Nano periodic mesoporous organic silicon oxide material and its synthetic method and its use
  • Nano periodic mesoporous organic silicon oxide material and its synthetic method and its use
  • Nano periodic mesoporous organic silicon oxide material and its synthetic method and its use

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Surfactant Brij76[C 18 h 37 (OCH 2 CH 2 ) 10 OH], Silicone BTEB[(C 2 h 5 O) 3 Si-C 6 h 4 -Si(OC 2 h 5 ) 3 , hydrochloric acid (HCl) and water at room temperature in the following molar ratio Brij76: H 2 O:HCl:BTEB=0.11:222:3.2:0.56 mixed. Specifically, Brij 76, H 2 O and HCl were pre-stirred at 323K for 12 hours, then BTEB was added to continue stirring for 12 hours, and then hydrothermally aged at 363K for 24 hours. After filtration, washing, and vacuum drying at 373K for 10 hours, the surfactant (350 mL / g) was extracted with 1M HCl / ethanol solution, washed with absolute ethanol, and finally the PMO material DDB1 was obtained in vacuum for 10 hours. With 0.12ml of 0.05g / mL PdCl 2Immerse 0.1g carrier in aqueous solution for 24h, dry in 373K oven, use 10V%H at 473K 2 / N 2 The Pd / DDB1 catalyst was prepared by reduction activation for 3h. 0.1g catalyst was added to the mixture containing 0.1mL iodobenzene (PhI), 2mL water, and 0.22g HCOONa (reducing agent...

Embodiment 2

[0035] Orthoethylsilicate (TEOS), cetyltrimethylammonium bromide (CTAB), sodium hydroxide (NaOH), phenyltrimethoxysilane (PTES) and water at room temperature in the following molar ratio: CTMABr :NaOH:Si:H 2 O=0.12:0.5:1.0:130, wherein Si is TEOS, stirred for 24h, filtered, washed, dried in vacuum at 100°C for 10h, then extracted the surfactant with 1M HCl / ethanol solution, washed with absolute ethanol, and finally Ph-MCM-41 was obtained in vacuum for 10 hours. with 1.8ml of 1.67wt% PdCl 2 Immerse the carrier in the aqueous solution for 24 hours, dry it in a 373K oven, and use 10V%H at 200°C 2 / N 2 The Pd / Ph-MCM-41 catalyst was prepared by reduction activation for 3h. The iodobenzene Ullmann reaction was carried out in a 50 mL round bottom flask equipped with a condenser. Mix 0.91g of iodobenzene (PhI), 10mL of water, 0.5g of catalyst, 1.10g of HCOONa (reducing agent) and 1.4g of KOH, and reflux at a constant temperature of 373K for 10h under electromagnetic stirring. Th...

Embodiment 3

[0037] Orthoethylsilicate (TEOS), cetyltrimethylammonium bromide (CTAB), sodium hydroxide (NaOH), phenyltrimethoxysilane (PTES) and water at room temperature in the following molar ratio: CTMABr :NaOH:Si:H 2 O=0.12:0.5:1.0:130, wherein Si=TEOS+PTES, PTES:TEOS=3:7 mixed, stirred for 24h, filtered, washed, vacuum dried at 373K for 10h, and then extracted with 1M HCl / ethanol solution for surface activity agent, then washed with absolute ethanol, and finally obtained Ph-MCM-41 in vacuum for 10 hours. With 1.8ml of 1.67wt% PdCl 2 Immerse the carrier in the aqueous solution for 24 hours, dry it in a 373K oven, and use 10V%H at 473K 2 / N 2 The Pd / Ph-MCM-41 catalyst was prepared by reduction activation for 3h. The iodobenzene Ullmann reaction was carried out in a 50 mL round bottom flask equipped with a condenser. Mix 0.91g of iodobenzene (PhI), 10mL of water, 0.5g of catalyst, 1.10g of HCOONa (reducing agent) and 1.4g of KOH, and reflux at a constant temperature of 373K for 10h ...

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Abstract

The present invention discloses one kind of nanometer periodical mesoporous organic silicon oxide material and its synthesis process and application as carrier for supporting Pd catalyst used in water phase iodobenzene coupling reaction. The material has pore size of 1.8-3.9 nm, pore volume of 0.3-1 cu cm/g and specific surface area of 800-1000 sq m/g. When the supported catalyst is used in the water phase iodobenzene coupling reaction, the supported catalyst has catalytic activity higher than that of Ph-MCM-41 supported catalyst prepared with no-phenyl radical modification MCM-41 and through copolymerization. The material is used in high efficiency heterogeneous catalyst, and has simple preparation process and no toxic and harmful matter.

Description

technical field [0001] The invention relates to a heterogeneous nanostructure catalyst carrier used in an organic reaction in a water solvent and its synthesis method and application in a chemical reaction, in particular to a phenyl-containing nano-periodic mesoporous organic silicon oxide material and its The synthesis method and the application of its supported Pd catalyst in catalyzing Ullmann coupling reaction in aqueous phase. Background technique [0002] In recent years, mesoporous molecular sieve materials have been extensively studied, and their high specific surface area and large pore size are conducive to obtaining highly dispersed supported catalysts, and the pore size and pore surface chemical properties of the catalyst can be adjusted. Among them, periodic mesoporous organosilicon materials Referred to as PMOs (periodic mesoporous organosilicas), the organic groups exist in the pore walls of the material and the organic functional groups are evenly distributed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J32/00B01J23/44C07C1/26C07C15/14C08G77/00
Inventor 万颖张蝶青熊明文李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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