Aryl halide to olefin arylation carrying bimetallic catalyst, and its preparing method

A technology of bimetallic catalyst and aryl halide is applied in the field of supported bimetallic catalyst and its preparation, and achieves the effects of easy separation, high catalytic activity and good stability

Inactive Publication Date: 2005-12-21
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Bimetallic or multimetallic catalysts are very common in catalytic chemistry research and industrial applications. This is because the interaction of bimetallic or multimetallic catalysts will have a significant impact on the activity and selectivity of the catalyst, but supported bimetallic catalysts in Heck The application in the reaction has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Weigh nickel nitrate trihydrate 0.0248g, add water 10ml, stir to dissolve; add activated carbon (BET specific surface area is 533.044m 2 / g) 1g, stir evenly; add 0.8ml of 0.01238g / ml palladium chloride hydrochloric acid solution, stir and impregnate for 1.5h; add dropwise 4ml of 3% potassium borohydride solution for reduction, and continue stirring for 2h after adding; filter, wash with water, Dry in an oven at 105°C overnight to prepare a 1%Pd-0.5%Ni / C catalyst.

Embodiment 2

[0040] Weigh 0.1486g of nickel nitrate hexahydrate, add 10ml of water, stir to dissolve; add 0.4ml of hydrochloric acid solution of 0.01238g / ml palladium chloride, stir well; add activated carbon (BET specific surface area is 533.044m 2 / g) 1g, stirring and impregnating for 1.5h; dropwise adding 5% potassium borohydride solution until the speed of bubble generation slows down significantly, consumes about 5ml of 5% potassium borohydride solution, continues to drop 0.5ml of 5% potassium borohydride solution, and drops Continue stirring for 2 hours; filter, wash with water, and dry overnight in an oven at a temperature of 105° C. to obtain a 0.5% Pd-3.0% Ni / C catalyst. XPS data shows that in the prepared catalyst, all Pd is Pd 0 , Ni has two oxidation states, Ni 0 and Ni 2+ , Ni 0 / Ni 2+ The ratio is approximately 1:3; in the XRD pattern, there is no obvious metal diffraction peak except for the carrier activated carbon.

Embodiment 3

[0042] Weigh 0.1481g of cobalt nitrate hexahydrate, add 10ml of water, stir to dissolve; add 0.4ml of hydrochloric acid solution of 0.01238g / ml palladium chloride, stir well; add activated carbon (BET specific surface area is 533.044m 2 / g) 1g, stirring and impregnating for 1.5h; dropwise adding 5% potassium borohydride solution until the speed of bubble generation slows down significantly, consumes about 5.2ml of 5% potassium borohydride solution, continues to drop 0.5ml of 5% potassium borohydride solution, dropwise Continue to stir for 2 hours; filter, wash with water, and dry overnight in an oven at a temperature of 105° C. to obtain a 0.5% Pd-3.0% Co / C catalyst. XPS data shows that in the prepared catalyst, all Pd is Pd 0 , the oxidation state of Co is different, Co has two oxidation states, Co 0 and Co 2+ ,Co 0 / Co 2+ The ratio is 2:3; in the XRD spectrum, there is no obvious metal diffraction peak except for the carrier activated carbon.

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Abstract

The invention relates to a kind of supported bimetallic complex catalyst of arylation to alkene by aryl halogenide and its preparing method. The catalyst contains precious metal Pd and / or base metal Cu, or Mo, or Ni, or Co, or Mn and carrier; the weight ratio of content of precious metal Pd counted as Pd and added carrier is 0.1% - 2.0%; the ratio of content of base metal counted as metal and added carrier is 0.5% - 10%. On the basis of precious metal Pd, add the other base metal Cu, or Mo, or Ni, or Co, or Mn; using chemical reduction method, prepare supported bimetallic complex catalyst used in Heck reaction; the watery solution concentration of reducing agent is 0.5% - 10%. The invention has following advantages: it has high catalyzing activeness, and short reacting time; it reduces the Pd dosage, and is easy to realize separation of output and catalyst.

Description

1. Technical field [0001] The invention relates to a metal catalyst, in particular to a supported bimetallic catalyst for arylation of olefins with aryl halides and a preparation method thereof. 2. Background technology [0002] The reaction of aryl halides and olefins to generate aryl olefins under the action of a catalyst is generally called the Heck reaction. The Heck reaction is a new type of carbon-carbon bond formation reaction. The carbon-carbon formation reaction is the basic reaction for building molecular structures in organic synthesis, and plays a very important role in organic synthesis. In the Heck reaction, since most functional groups, such as alcohols, ethers, ketones, esters, etc., can be tolerated no matter whether they are on halides or on alkenes, and the reaction products have high regioselectivity and stereoselectivity, Therefore, the Heck reaction is widely used in organic synthesis. [0003] The Heck reaction was independently discovered by Richard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/64
Inventor 崔名全张昭张明俊
Owner SICHUAN UNIV
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