Preparation method of MnFe2O4-TiO2-graphene aerogel

Abstract

The invention discloses a preparation method of MnFe2O4-TiO2-graphene aerogel. The preparation method comprises the following steps: (1), mixing a graphene oxide aqueous solution with absolute ethyl alcohol, then carrying out ultrasonic treatment, y adding ferric nitrate and manganous nitrate salt solutions, then adding polyethyleneimine for ultrasonic treatment, and finally adding tetrabutyl titanate for ultrasonic treatment to form a good dispersion liquid; (2), transferring the dispersion liquid into a high-temperature and high-pressure reaction kettle for reaction; and (3), after finishingof the reaction, taking out the sample, soaking the sample in ammonia water (10v / v%), and soaking the sample in 20% ethanol before freeze drying to prepare MnFe2O4-TiO2-graphene aerogel. According tothe preparation method, aerogel is synthesized through a one-step hydrothermal method, reduction of graphene oxide is promoted through addition of polyethyleneimine, self-assembly of the aerogel is easier to complete, and amino is introduced to enhance the mechanical strength of the aerogel. The preparation method of the aerogel is simple and convenient, the aerogel serving as a catalyst is easyto recycle, secondary pollution is reduced, and the visible light utilization rate is increased.

Description

technical field

[0001] The present invention relates to a kind of one-step synthetic MnFe 2 o 4 -TiO 2 -The preparation method of graphene airgel belongs to the field of catalyst preparation. Background technique

[0002] With the development of industry, more and more refractory organic substances are produced and accumulated. Traditional methods such as adsorption and coagulation are only a physical separation of organic matter, and have not completed the degradation of refractory organic matter. An efficient method is needed to deal with the increasingly serious water pollution problem.

[0003] Photocatalytic technology has attracted more and more attention because of its non-selectivity to organic matter, its ability to completely degrade organic matter, and the use of solar energy. However, photocatalytic technology also faces the problems of long degradation cycle and low efficiency. Therefore, it is of great significance to choose a composite system to improve ef...

Examples

Embodiment 1

[0031] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2h, and prepare a 4mg / mL graphene oxide aqueous solution;

[0032] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 30min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 30 minutes to form solution A;

[0033] (3) Measure 1mL polyethyleneimine aqueous solution (40mg / mL) and add solution A to ultrasonic for 30min, pH to 10.5, then add 0.19mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonically for 30min , forming a good dispersion;

[0034] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0035] (5) After the reaction is over, take out the sample after the reactor is cooled to room tempera...

Embodiment 2

[0041] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2h, and prepare a 4mg / mL graphene oxide aqueous solution;

[0042] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 30min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 30 minutes to form solution A;

[0043] (3) Measure 1mL polyethyleneimine aqueous solution (30mg / mL) and add solution A to ultrasonic for 30min, pH to 10, then add 0.125mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonicate for 30min , forming a good dispersion;

[0044] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0045] (5) After the reaction is over, take out the sample after the reaction kettle is cooled to room t...

Embodiment 3

[0048] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2 hours, and prepare a 4mg / mL graphene oxide aqueous solution;

[0049] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 20min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 50 minutes to form solution A;

[0050] (3) Measure 1mL polyethyleneimine aqueous solution (30mg / mL) and add solution A to ultrasonic for 30min, pH to 10, then add 0.19mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonically for 30min , forming a good dispersion;

[0051] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0052] (5) After the reaction is over, take out the sample after the reaction kettle is cooled to r...

technical field

[0001] The present invention relates to a kind of one-step synthetic MnFe 2 o 4 -TiO 2 -The preparation method of graphene airgel belongs to the field of catalyst preparation. Background technique

[0002] With the development of industry, more and more refractory organic substances are produced and accumulated. Traditional methods such as adsorption and coagulation are only a physical separation of organic matter, and have not completed the degradation of refractory organic matter. An efficient method is needed to deal with the increasingly serious water pollution problem.

[0003] Photocatalytic technology has attracted more and more attention because of its non-selectivity to organic matter, its ability to completely degrade organic matter, and the use of solar energy. However, photocatalytic technology also faces the problems of long degradation cycle and low efficiency. Therefore, it is of great significance to choose a composite system to improve ef...

Examples

Embodiment 1

[0031] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2h, and prepare a 4mg / mL graphene oxide aqueous solution;

[0032] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 30min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 30 minutes to form solution A;

[0033] (3) Measure 1mL polyethyleneimine aqueous solution (40mg / mL) and add solution A to ultrasonic for 30min, pH to 10.5, then add 0.19mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonically for 30min , forming a good dispersion;

[0034] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0035] (5) After the reaction is over, take out the sample after the reactor is cooled to room tempera...

Embodiment 2

[0041] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2h, and prepare a 4mg / mL graphene oxide aqueous solution;

[0042] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 30min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 30 minutes to form solution A;

[0043] (3) Measure 1mL polyethyleneimine aqueous solution (30mg / mL) and add solution A to ultrasonic for 30min, pH to 10, then add 0.125mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonicate for 30min , forming a good dispersion;

[0044] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0045] (5) After the reaction is over, take out the sample after the reaction kettle is cooled to room t...

Embodiment 3

[0048] (1) Place 0.4g graphene oxide in 100mL ultrapure water, use an ultrasonic crusher at a power of 270W, crush for 2 hours, and prepare a 4mg / mL graphene oxide aqueous solution;

[0049] (2) Add 12.5mL (1) graphene oxide aqueous solution and 12.5mL absolute ethanol to the beaker for 20min, then dissolve 0.0913g ferric nitrate nonahydrate and 0.0285g manganese nitrate tetrahydrate in 5mL ultrapure water, pour Pour into a beaker and sonicate for 50 minutes to form solution A;

[0050] (3) Measure 1mL polyethyleneimine aqueous solution (30mg / mL) and add solution A to ultrasonic for 30min, pH to 10, then add 0.19mL tetrabutyl titanate to 5mL absolute ethanol, add to the above solution and ultrasonically for 30min , forming a good dispersion;

[0051] (4) Transfer the above dispersion to a 50mL high-temperature and high-pressure reactor, and react in an oven at 180°C for 24h;

[0052] (5) After the reaction is over, take out the sample after the reaction kettle is cooled to r...

Images