Lignosulfonate-phenolic resin based carbon aerogel microsphere as well as preparation method and application thereof

Abstract

The invention discloses a lignosulfonate phenolic resin based carbon aerogel microsphere as well as a preparation method and application thereof. The preparation method comprises the steps of dissolving lignosulfonate, a phenolic compound, an aldehyde compound and a polyamine compound in water to obtain a water phase; mixing the water phase with a non-water-soluble oil phase, carrying out polymerization reaction under a stirring condition, filtering and separating after the polymerization reaction is finished, and carrying out water seal aging and drying on the obtained solid product to obtaindry gel microspheres; carrying out carbonization treatment on the dry gel microspheres, and washing to obtain the lignosulfonate phenolic resin-based carbon aerogel microspheres which are small in macroscopic particle size, developed in microscopic pore structure and large in specific surface area and contain polar groups and a molecular imprinting-like specific structure. The carbon aerogel microsphere material can be used for selective and efficient adsorption of heavy metals, and is especially suitable for remediation of heavy metal contaminated soil. The preparation raw materials of the carbon aerogel microsphere are wide in source and low in cost, so that large-scale production and application are facilitated.

Description

technical field

[0001] The invention relates to a carbon airgel microsphere material, in particular to a lignosulfonate synthesized by oil-water two-phase suspension polymerization with microsphere shape, large specific surface area, well-developed pores, and molecularly imprinted specific structure -The phenolic resin-based carbon airgel microsphere material also relates to the application of the lignosulfonate-phenolic resin-based carbon airgel microsphere material in the remediation of heavy metal polluted soil, which belongs to the field of ecological environment management. Background technique

[0002] Different from common bulk aerogels, microspherical aerogels, or airgel microspheres, also known as microaerogels, are a special new material that is constructed of both nanoscale materials and micron Level size (usually between 1 and 1000 μm), and also has the same three-dimensional network porous structure as the macroscopic bulk aerogel. The preparation of aerogels i...

Examples

Embodiment 1

[0037] Embodiment 1 (control experiment)

[0038] In a 250mL three-necked flask, add 12.98g of resorcinol, 4g of hexamethylenetetramine, 18.97ml of formaldehyde, add deionized water to make the volume to 40ml, stir evenly, pour 120ml of peanut oil, and use 300r / min continue to stir and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, the residual peanut oil on the surface was washed away, and after vacuum drying, it was heated in a tube furnace at 800°C for 4 hours under a nitrogen atmosphere. After cooling, the black solid was taken out to obtain carbon airgel microspheres without imprinting. The carbonization yield of the carbon airgel is: 53.5%, the average particle size is 120μm, and the specific surface area is 470m 2 / ...

Embodiment 2

[0040] In a 250mL three-necked flask, add 8.98g of resorcinol, 4.02g of sodium lignosulfonate, 4g of hexamethylenetetramine, and 18.97ml of formaldehyde, add deionized water to make it 40ml, and stir evenly. Pour in 120ml of peanut oil, continue stirring at 450r / min, and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, wash off the residual peanut oil on the surface. After vacuum drying, heat in a tube furnace at 300°C for 4 hours in a nitrogen atmosphere. After cooling, take out the black solid and wash it with pure water until the pH is constant. glue microspheres. The carbonization yield of the carbon airgel is: 51.3%, the average particle size is 78μm, and the specific surface area is 615m 2 / g, average pore diameter: 131...

Embodiment 3

[0043] In a 250mL three-necked flask, add 9.02g of resorcinol, 3.98g of zinc lignosulfonate, 2g of hexamethylenetetramine, 18.97ml of formaldehyde, add deionized water to make it 40ml, and stir evenly. Pour in 120ml peanut oil, continue stirring at 600r / min, and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, wash off the residual peanut oil on the surface. After vacuum drying, heat in a tube furnace at 800°C for 4 hours under a nitrogen atmosphere. After cooling, take out the black solid, wash with 1mol / L hydrochloric acid three times to remove zinc ions, and then wash with pure water until the pH is constant. That is, carbon airgel microspheres with zinc ion imprinting are obtained. The carbonization yield of the carbon air...

technical field

[0001] The invention relates to a carbon airgel microsphere material, in particular to a lignosulfonate synthesized by oil-water two-phase suspension polymerization with microsphere shape, large specific surface area, well-developed pores, and molecularly imprinted specific structure -The phenolic resin-based carbon airgel microsphere material also relates to the application of the lignosulfonate-phenolic resin-based carbon airgel microsphere material in the remediation of heavy metal polluted soil, which belongs to the field of ecological environment management. Background technique

[0002] Different from common bulk aerogels, microspherical aerogels, or airgel microspheres, also known as microaerogels, are a special new material that is constructed of both nanoscale materials and micron Level size (usually between 1 and 1000 μm), and also has the same three-dimensional network porous structure as the macroscopic bulk aerogel. The preparation of aerogels i...

Examples

Embodiment 1

[0037] Embodiment 1 (control experiment)

[0038] In a 250mL three-necked flask, add 12.98g of resorcinol, 4g of hexamethylenetetramine, 18.97ml of formaldehyde, add deionized water to make the volume to 40ml, stir evenly, pour 120ml of peanut oil, and use 300r / min continue to stir and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, the residual peanut oil on the surface was washed away, and after vacuum drying, it was heated in a tube furnace at 800°C for 4 hours under a nitrogen atmosphere. After cooling, the black solid was taken out to obtain carbon airgel microspheres without imprinting. The carbonization yield of the carbon airgel is: 53.5%, the average particle size is 120μm, and the specific surface area is 470m 2 / ...

Embodiment 2

[0040] In a 250mL three-necked flask, add 8.98g of resorcinol, 4.02g of sodium lignosulfonate, 4g of hexamethylenetetramine, and 18.97ml of formaldehyde, add deionized water to make it 40ml, and stir evenly. Pour in 120ml of peanut oil, continue stirring at 450r / min, and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, wash off the residual peanut oil on the surface. After vacuum drying, heat in a tube furnace at 300°C for 4 hours in a nitrogen atmosphere. After cooling, take out the black solid and wash it with pure water until the pH is constant. glue microspheres. The carbonization yield of the carbon airgel is: 51.3%, the average particle size is 78μm, and the specific surface area is 615m 2 / g, average pore diameter: 131...

Embodiment 3

[0043] In a 250mL three-necked flask, add 9.02g of resorcinol, 3.98g of zinc lignosulfonate, 2g of hexamethylenetetramine, 18.97ml of formaldehyde, add deionized water to make it 40ml, and stir evenly. Pour in 120ml peanut oil, continue stirring at 600r / min, and start heating. When the reaction reaches the set temperature, start timing. The reaction was carried out at a reaction temperature of 80° C. for 100 minutes. After the reaction, brown solid particles appeared. After filtration, the yellow solid was taken out and aged at 80°C for 5 days. After aging, wash off the residual peanut oil on the surface. After vacuum drying, heat in a tube furnace at 800°C for 4 hours under a nitrogen atmosphere. After cooling, take out the black solid, wash with 1mol / L hydrochloric acid three times to remove zinc ions, and then wash with pure water until the pH is constant. That is, carbon airgel microspheres with zinc ion imprinting are obtained. The carbonization yield of the carbon air...

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