Method for preparing carbon nanospheres through cooperation of pressure and dispersing agent

Abstract

The invention relates to a carbon nanosphere preparation technology, in particular to a method for preparing carbon nanospheres through cooperation of pressure and a dispersing agent, and solves the problems that in an existing carbon nanosphere synthesis method, carbon spheres are prone to adhesion, and the yield is low. The method comprises the following steps: S1, preparing a mixed solution ofglucose and a dispersing agent, wherein the dispersing agent is sodium polyphosphate, and the mass ratio of glucose to sodium polyphosphate is 1: 0.003-1: 0.01; s2, putting the mixed solution preparedin the step S1 into a high-pressure kettle, sealing the high-pressure kettle, introducing inert gas through a gas inlet, and pressurizing to enable the initial pressure in the kettle to be 0.5-4.0 MPa; S3, heating the autoclave in the step S2 to carry out hydrothermal synthesis reaction to obtain a solution of carbon nanospheres; and S4, washing and drying the carbon nanosphere solution obtainedin the step S3 to obtain the carbon nanospheres. According to the method, the carbon nanospheres with adjustable particle size of 75-96nm, good dispersity, uniform size and high yield can be obtainedby changing the pressure and the dosage of the dispersing agent, and theoretical and technical supports are provided for large-scale industrial production.

Description

technical field

[0001] The invention relates to the preparation technology of nano carbon spheres, in particular to a method for synergistically preparing nano carbon spheres by pressure and a dispersant. Background technique

[0002] Carbon nanospheres are widely used in catalysis or catalyst support, adsorption, electrochemistry, biomedicine and other fields due to their small particle size (<100nm), regular spherical morphology and abundant surface functional groups. Compared with micro-nano carbon spheres, nano-carbon spheres have a higher specific surface area and more abundant surface functional groups, and exhibit superior performance when used as catalyst supports, electrode materials and adsorption materials.

[0003] High-quality preparation of carbon nanospheres still faces great challenges, which is attributed to the synthesis mechanism of carbon spheres: firstly, glucose is decomposed to generate 5-hydroxymethylfurfural, various organic acids and other compou...

Examples

Embodiment 1

[0030] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0031] S1, configure the concentration of glucose solution to be 1.0M, the amount of dispersant poly(4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) is 1% of the amount of glucose, and stir to obtain a mixed solution;

[0032] S2. Take 33mL of the mixed solution configured in step S1 and put it into a 100mL autoclave. After the autoclave is sealed, nitrogen gas is introduced through the air inlet so that the initial pressure in the still is 4.0MPa;

[0033] S3. Heating the autoclave in step S2 to 200° C. and then keeping the temperature for 3 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0034] S4. Separate the nano-carbon sphere solution obtained in S3 at a centrifugal rate of 18000r / min for 30 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, and then u...

Embodiment 2

[0037] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0038] S1, configure the concentration of glucose solution to be 0.8M, the amount of dispersant poly(4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) is 0.5% of the amount of glucose, and stir to obtain a mixed solution;

[0039] S2. Take 60 mL of the mixed solution configured in step S1 and put it into a 100 mL autoclave. After the autoclave is sealed, nitrogen gas is introduced through the air inlet so that the initial pressure in the still is 3.0 MPa;

[0040] S3. Heating the autoclave in step S2 to 180° C. and then keeping the temperature for 6 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0041] S4. Separate the nano-carbon sphere solution obtained in S3 with a centrifugation rate of 15000r / min for 20 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, ...

Embodiment 3

[0044] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0045] S1, configure the concentration of glucose solution to be 0.7M, the amount of dispersant poly(4-styrenesulfonic acid-copolymerization-maleic acid) sodium salt (PSSMA) is 0.8% of the amount of glucose, and stir to obtain a mixed solution;

[0046] S2, get 50mL of the mixed solution configured in step S1, put it into a 100mL autoclave, and after the autoclave is sealed, feed nitrogen through the air inlet so that the initial pressure in the still is 2.5MPa;

[0047] S3. Heating the autoclave in step S2 to 200° C. and then keeping the temperature for 3 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0048] S4. Separate the nano-carbon sphere solution obtained in S3 at a centrifugal rate of 20,000 r / min for 50 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, and the...

technical field

[0001] The invention relates to the preparation technology of nano carbon spheres, in particular to a method for synergistically preparing nano carbon spheres by pressure and a dispersant. Background technique

[0002] Carbon nanospheres are widely used in catalysis or catalyst support, adsorption, electrochemistry, biomedicine and other fields due to their small particle size (<100nm), regular spherical morphology and abundant surface functional groups. Compared with micro-nano carbon spheres, nano-carbon spheres have a higher specific surface area and more abundant surface functional groups, and exhibit superior performance when used as catalyst supports, electrode materials and adsorption materials.

[0003] High-quality preparation of carbon nanospheres still faces great challenges, which is attributed to the synthesis mechanism of carbon spheres: firstly, glucose is decomposed to generate 5-hydroxymethylfurfural, various organic acids and other compou...

Examples

Embodiment 1

[0030] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0031] S1, configure the concentration of glucose solution to be 1.0M, the amount of dispersant poly(4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) is 1% of the amount of glucose, and stir to obtain a mixed solution;

[0032] S2. Take 33mL of the mixed solution configured in step S1 and put it into a 100mL autoclave. After the autoclave is sealed, nitrogen gas is introduced through the air inlet so that the initial pressure in the still is 4.0MPa;

[0033] S3. Heating the autoclave in step S2 to 200° C. and then keeping the temperature for 3 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0034] S4. Separate the nano-carbon sphere solution obtained in S3 at a centrifugal rate of 18000r / min for 30 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, and then u...

Embodiment 2

[0037] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0038] S1, configure the concentration of glucose solution to be 0.8M, the amount of dispersant poly(4-styrenesulfonic acid-co-maleic acid) sodium salt (PSSMA) is 0.5% of the amount of glucose, and stir to obtain a mixed solution;

[0039] S2. Take 60 mL of the mixed solution configured in step S1 and put it into a 100 mL autoclave. After the autoclave is sealed, nitrogen gas is introduced through the air inlet so that the initial pressure in the still is 3.0 MPa;

[0040] S3. Heating the autoclave in step S2 to 180° C. and then keeping the temperature for 6 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0041] S4. Separate the nano-carbon sphere solution obtained in S3 with a centrifugation rate of 15000r / min for 20 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, ...

Embodiment 3

[0044] A high-efficiency preparation method of hydrothermal nano-carbon spheres, comprising the following steps:

[0045] S1, configure the concentration of glucose solution to be 0.7M, the amount of dispersant poly(4-styrenesulfonic acid-copolymerization-maleic acid) sodium salt (PSSMA) is 0.8% of the amount of glucose, and stir to obtain a mixed solution;

[0046] S2, get 50mL of the mixed solution configured in step S1, put it into a 100mL autoclave, and after the autoclave is sealed, feed nitrogen through the air inlet so that the initial pressure in the still is 2.5MPa;

[0047] S3. Heating the autoclave in step S2 to 200° C. and then keeping the temperature for 3 hours. After the reaction, naturally cool to room temperature to obtain a carbon nanosphere solution;

[0048] S4. Separate the nano-carbon sphere solution obtained in S3 at a centrifugal rate of 20,000 r / min for 50 minutes, centrifuge with deionized water, and ultrasonically disperse and wash three times, and the...

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