A kind of preparation method of catalyst and method for catalytic preparation of 2,2-bipyridine

Abstract

The invention discloses a preparation method of a catalyst and belongs to the field of preparation and application of catalysts. The preparation method comprises the following steps of: a) in the presence of inert gas, mixing acetylacetone, cobalt hydroxide, benzene and / or benzene derivative, then distilling moisture until the moisture content of reflux is less than 300ppm, so as to obtain a solution A containing cobalt acetylacetonate, and cooling to the temperature below -10 DEG C for later use; b) in the presence of inert gas, mixing cyclopentadiene, 1,5-cyclooctadiene, benzene and / or benzene derivative, cooling to the temperature below -10 DG C, adding triethyl aluminum, and uniformly mixing, so as to obtain a solution B is obtained; and c) slowly adding the solution B into the solution A at the temperature below 0 DEG C, stirring, heating to 25 DEG C, reacting for 3-5 hours, and filtering, wherein the obtained filtrate is the catalyst benzene and / or benzene derivative solution of 1,5-cyclooctadiene cyclopentadienyl cobalt. The invention also discloses a method for preparing 2,2-dipyridyl by utilizing the catalyst.

Description

technical field

[0001] The invention belongs to the field of catalyst preparation and application, and in particular relates to a catalyst preparation method and a method for catalytically preparing 2,2-bipyridine. Background technique

[0002] 2,2-Bipyridyl is an essential raw material for the production of the herbicide diquat, and is also an intermediate of other chemical raw materials, widely used in the synthesis of pesticides, medicines, spices and dyes. At the same time, it is also a metal chelating agent, which can be used in metal color developing agents, and has a good market prospect.

[0003] At present, the production methods of 2,2-bipyridine mainly include halogenated pyridine coupling and pyridine dehydrogenation. Both methods have problems such as large environmental pollution and difficult wastewater treatment, and it is difficult to expand the production scale. According to Synthesis of 2,2 ′-Bipyridines: Versatile Building Blocks for Sexy Architectures a...

Examples

Embodiment 1

[0018] A preparation method containing a catalyst, comprising the following steps:

[0019] a) Into the reaction kettle with nitrogen protection, add 12 parts of acetylacetone and 500 parts of toluene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 11 parts of cobalt hydroxide, and raise the temperature until the solvent starts to evaporate through the rectification tower Reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is divided into water in the water separator, the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, and the top water The azeotrope with benzene and water is condensed and then returned to the water separator, and the bottom benzene and / or benzene derivatives are returned to the reaction system to continue to carry water until the moisture content in the reflux night is less...

Embodiment 2

[0024] A preparation method containing a catalyst, comprising the following steps:

[0025] a) Pass nitrogen protection into the reaction kettle, add 12 parts of acetylacetone and 500 parts of xylene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 12 parts of cobalt hydroxide, and raise the temperature until the solvent begins to pass through the rectification tower Evaporation and reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is separated into water in the water separator, and the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, the top of the tower Water, benzene, and water azeotrope are condensed and then returned to the water separator, and the benzene and / or benzene derivatives at the bottom of the tower are returned to the reaction system to continue to carry water until the moist...

Embodiment 3

[0030] A preparation method containing a catalyst, comprising the following steps:

[0031] a) Put nitrogen protection in the reaction kettle, add 12 parts of acetylacetone and 500 parts of benzene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 13 parts of cobalt hydroxide, and heat up until the solvent starts to evaporate through the rectification tower Reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is divided into water in the water separator, the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, and the top water The azeotrope with benzene and water is condensed and then returned to the water separator, and the bottom benzene and / or benzene derivatives are returned to the reaction system to continue to carry water until the moisture content in the reflux night is less than 300ppm, and...

technical field

[0001] The invention belongs to the field of catalyst preparation and application, and in particular relates to a catalyst preparation method and a method for catalytically preparing 2,2-bipyridine. Background technique

[0002] 2,2-Bipyridyl is an essential raw material for the production of the herbicide diquat, and is also an intermediate of other chemical raw materials, widely used in the synthesis of pesticides, medicines, spices and dyes. At the same time, it is also a metal chelating agent, which can be used in metal color developing agents, and has a good market prospect.

[0003] At present, the production methods of 2,2-bipyridine mainly include halogenated pyridine coupling and pyridine dehydrogenation. Both methods have problems such as large environmental pollution and difficult wastewater treatment, and it is difficult to expand the production scale. According to Synthesis of 2,2 ′-Bipyridines: Versatile Building Blocks for Sexy Architectures a...

Examples

Embodiment 1

[0018] A preparation method containing a catalyst, comprising the following steps:

[0019] a) Into the reaction kettle with nitrogen protection, add 12 parts of acetylacetone and 500 parts of toluene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 11 parts of cobalt hydroxide, and raise the temperature until the solvent starts to evaporate through the rectification tower Reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is divided into water in the water separator, the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, and the top water The azeotrope with benzene and water is condensed and then returned to the water separator, and the bottom benzene and / or benzene derivatives are returned to the reaction system to continue to carry water until the moisture content in the reflux night is less...

Embodiment 2

[0024] A preparation method containing a catalyst, comprising the following steps:

[0025] a) Pass nitrogen protection into the reaction kettle, add 12 parts of acetylacetone and 500 parts of xylene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 12 parts of cobalt hydroxide, and raise the temperature until the solvent begins to pass through the rectification tower Evaporation and reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is separated into water in the water separator, and the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, the top of the tower Water, benzene, and water azeotrope are condensed and then returned to the water separator, and the benzene and / or benzene derivatives at the bottom of the tower are returned to the reaction system to continue to carry water until the moist...

Embodiment 3

[0030] A preparation method containing a catalyst, comprising the following steps:

[0031] a) Put nitrogen protection in the reaction kettle, add 12 parts of acetylacetone and 500 parts of benzene with strong stirring, control the temperature of the reaction system below 10°C, slowly add 13 parts of cobalt hydroxide, and heat up until the solvent starts to evaporate through the rectification tower Reflux, using benzene and / or benzene derivatives and water to form an azeotropic reaction liquid for continuous evaporation and dehydration, the condensate is divided into water in the water separator, the upper layer of benzene and / or benzene derivatives is returned to the rectification tower, and the top water The azeotrope with benzene and water is condensed and then returned to the water separator, and the bottom benzene and / or benzene derivatives are returned to the reaction system to continue to carry water until the moisture content in the reflux night is less than 300ppm, and...