Preparation method of lignin-based porous carbon material

Abstract

The invention belongs to the field of carbon material preparation, and particularly relates to a preparation method of a lignin-based porous carbon material. Under the oxidation action of low-concentration hydrogen peroxide, ozone blowing during low-temperature carbonization and a low-temperature carbonization charking process are combined, so that the orderliness and regularity of lignin molecules are improved, the oxidation of unsaturated bonds of lignin is promoted, and the activation of an activating agent melamine pyrophosphate is carried out, so that small molecules can be quickly removed during high-temperature cracking, the charking time is shortened, the yield of the carbon material is increased, and the obtained carbon material is more excellent in performance.

Description

Technical field

[0001] The invention belongs to the field of carbon material preparation, and specifically relates to a preparation method of a lignin-based porous carbon material.Background technique

[0002] Lignin (Lig) is an amorphous polymer formed by connecting three kinds of phenylpropane as the basic unit through ester bond and carbon-carbon bond. Its carbon chain and benzene ring contain hydroxyl, carboxyl, methoxy, carbonyl, carbon-carbon The existence of functional groups such as double bonds and benzene ring makes lignin possess a variety of chemical properties and can undergo various reactions such as alcoholysis, reduction, oxidation, hydrolysis, acylation, alkylation, polycondensation and copolymerization. At present, the application fields of lignin in my country are mainly concentrated in industrial fields such as resin products, concrete preparation, hydrogels and pesticides. As the only polymer containing a benzene ring structure in plant resources, lignin has the poten...

Examples

Embodiment 1

[0026]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) to make 100mL alkaline solution with water, then add 2g of melamine pyrophosphate, put it in a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow air into the tube furnace for 40 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this example was 17%, and the high-temperature carbonization time was 55 minutes.

Embodiment 2

[0028]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) and add water to make a 100mL alkaline solution, then add 6g of melamine pyrophosphate, put it into a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow air into the tube furnace for 40 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this embodiment was 26.8%, and the high-temperature carbonization time was 20 minutes.

Embodiment 3

[0030]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) to make 100mL alkaline solution with water, then add 2g of melamine pyrophosphate, put it in a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow into the tube furnace for 20 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this embodiment is 10%, and the high-temperature carbonization time is 60 minutes.

Technical field

[0001] The invention belongs to the field of carbon material preparation, and specifically relates to a preparation method of a lignin-based porous carbon material.Background technique

[0002] Lignin (Lig) is an amorphous polymer formed by connecting three kinds of phenylpropane as the basic unit through ester bond and carbon-carbon bond. Its carbon chain and benzene ring contain hydroxyl, carboxyl, methoxy, carbonyl, carbon-carbon The existence of functional groups such as double bonds and benzene ring makes lignin possess a variety of chemical properties and can undergo various reactions such as alcoholysis, reduction, oxidation, hydrolysis, acylation, alkylation, polycondensation and copolymerization. At present, the application fields of lignin in my country are mainly concentrated in industrial fields such as resin products, concrete preparation, hydrogels and pesticides. As the only polymer containing a benzene ring structure in plant resources, lignin has the poten...

Examples

Embodiment 1

[0026]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) to make 100mL alkaline solution with water, then add 2g of melamine pyrophosphate, put it in a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow air into the tube furnace for 40 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this example was 17%, and the high-temperature carbonization time was 55 minutes.

Embodiment 2

[0028]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) and add water to make a 100mL alkaline solution, then add 6g of melamine pyrophosphate, put it into a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow air into the tube furnace for 40 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this embodiment was 26.8%, and the high-temperature carbonization time was 20 minutes.

Embodiment 3

[0030]Take 3g of sodium hydroxide, 3g of lignin, 1g of hydrogen peroxide (concentration of 30%, AR) to make 100mL alkaline solution with water, then add 2g of melamine pyrophosphate, put it in a three-necked flask, magnetically stir for 6h, and ultrasonically disperse for 1h , And then spray drying (outlet temperature 100 ℃), the obtained powder is put into a tube furnace, using an odor generator to blow into the tube furnace for 20 minutes (ozone content about 3.33g), 190 ℃ low temperature carbonization for 2 hours, heating at It is calcined at a high temperature in a nitrogen atmosphere at a temperature of 850°C. The obtained carbon block is pickled, washed with water, pulverized with an ultrafine wet pulverizer, and finally vacuum dried for 12 hours to obtain the final product carbon material. The yield of the carbon material obtained in this embodiment is 10%, and the high-temperature carbonization time is 60 minutes.

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