Nano Pd catalyst and its preparation and application

A catalyst and nano-palladium technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as increased equipment investment and operating costs, health hazards for workers, and difficult product purification, etc., to achieve omission Solvent recovery, elimination of potential safety hazards, and the effect of eradicating organic solvents

Inactive Publication Date: 2006-12-27
淮北煤炭师范学院
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  • Abstract
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AI Technical Summary

Problems solved by technology

The usual synthetic method is to use substituted phenylboronic acid and substituted halogen (bromine and iodine) benzene as raw materials, under the catalysis of transition metal palladium complexes, in organic solvents such as triethylamine, diethylamine, tetrahydrofuran, N, N-di Complete (Suzuki Coupling Suzuki coupling reaction) in methyl formamide, this method technology is mature, but the use and discharge etc. of metal palladium and ligand cause environmental pollution in the production process; And metal palladium black can pollute product so that make It is difficult to purify the product; in addition, another disadvantage of this method is the use of a large amount of organic solvents, which need to be recycled, which increases equipment investment and operating costs, and pollutes the environment, causing harm to workers' health

Method used

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  • Nano Pd catalyst and its preparation and application

Examples

Experimental program
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Effect test

preparation example Construction

[0014] (1), preparation of catalyst

[0015] 1. Take 300-500ml of ethanol and add it to the reaction flask with a reflux condenser, add 17.7g of palladium chloride and 32.3g of polyvinyl alcohol under stirring, heat up after dissolving, react at 80°C for 2 hours, and the new ecological black nano palladium powder (average particle size 5nm) precipitated out and attached to polyvinyl alcohol. After the reaction is finished, the ethanol is evaporated to obtain the polyvinyl alcohol-supported nano-palladium catalyst.

[0016] 2. Take 300-500ml of ethylene glycol, 23g of palladium nitrate, 37g of sodium alginate, 75°C for 3 hours, and other operations are the same

Embodiment 1

[0018] 3. Take 300-500 ml of ethanol and propanol mixed alcohol, 22.4 g of palladium acetate, and 32.6 g of carboxymethyl cellulose, at 85° C. for 2 hours, and other operations are the same as in Example 1.

[0019] 4. Take 300-500 ml of propanol, 17.7 g of palladium chloride, and 32.3 g of polyethylene oxide, at 80° C. for 2 hours, and other operations are the same as in Example 1.

[0020] (2), the preparation of biphenyl compound

[0021] Now taking the preparation of p-toluene as an example, non-limiting examples are described as follows:

[0022] 5. Put 6L of tap water into the reaction kettle, add 50g of this catalyst (containing 10.6g, 0.1mol of palladium black) and equimolar (20ml) of iodobenzene, p-tolueneboronic acid and potassium carbonate under stirring, heat up, and react at 80°C for 3~ 4 hours. After the reaction is finished, cool down, let stand at room temperature and separate the layers, separate the water phase, and recycle it for reuse. The organic phase ...

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Abstract

Disclosed is a nano-palladium catalyst which is polymer loading nano-palladium catalyst produced by water-soluble inorganic palladium salt and water-soluble macromolecule in low-carbon alcohol at 60-90 DEG C. The preparation process is simple, activity of the catalyst is high and the catalyst can be used repeatedly. When using the catalyst to preparation biphenyl, solvent can be water, organic base can be replaced by inorganic base, the process is simplified and avoids more waste gas, liquid and solid, dosage of catalyst is few, purity of product is not less than 99.5 % and yield is not less than 95 %.

Description

1. Technical field [0001] The invention relates to a catalyst for organic synthesis and its preparation method and application, in particular to a nano-palladium catalyst, its preparation method and its application in coupling reaction preparation of biphenyl compounds. 2. Background technology [0002] Biphenyl compound is an important organic intermediate, which is widely used in the production of many fine chemicals such as materials, medicine, pesticides, and daily chemicals. The usual synthetic method is to use substituted phenylboronic acid and substituted halogen (bromine and iodine) benzene as raw materials, under the catalysis of transition metal palladium complexes, in organic solvents such as triethylamine, diethylamine, tetrahydrofuran, N, N-di Complete (Suzuki Coupling Suzuki coupling reaction) in methyl formamide, this method technology is mature, but the use and discharge etc. of metal palladium and ligand cause environmental pollution in the production proces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/00
Inventor 王磊李品华李洪基
Owner 淮北煤炭师范学院
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