Solvent-free hydrothermal preparation method of carbon material

A technology of carbon materials and hydrothermal method, which is applied in the field of preparation of solvent-free hydrothermal carbon materials, can solve the problems of complicated and time-consuming experimental operations, and achieve the effects of reducing experimental risks, good specific surface area, and saving centrifugal suction and drying

Active Publication Date: 2020-11-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Experimental operation is complicated and time-consuming

Method used

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  • Solvent-free hydrothermal preparation method of carbon material
  • Solvent-free hydrothermal preparation method of carbon material
  • Solvent-free hydrothermal preparation method of carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Take 1g of tannin, 1g of vanillin, and 2g of nano-calcium carbonate and mix them in a mortar. After fully grinding and mixing, add 4-5 drops of 0.5m dilute sulfuric acid to continue grinding, and grind the sample until the surface is wet.

[0027] (2) Transfer the ground sample in step (1) into a 50ml hydrothermal kettle, place it in a vacuum drying oven, and react at 180°C for 12 hours.

[0028] (3) Take out the carbon material precursor in step (2), transfer it into a quartz boat, place it in a tube furnace, and carbonize it in an atmosphere with a nitrogen flow rate of 100 ml / min. The heating rate is 2 °C / min, and the temperature is raised to 900 °C. , After 1.5 hours of heat preservation, cooling treatment.

[0029] (4) The sample obtained in step (3) was ground and pulverized, magnetically stirred with 0.5 m dilute hydrochloric acid for 6 hours, subjected to ultrasonic treatment for 2 hours and then filtered with suction, and the sample was dried in a blast dry...

Embodiment 2

[0032] (1) Take 1g of tannin, 1g of vanillin, and 3g of nano-calcium carbonate and mix them in a mortar. After fully grinding and mixing, add 4-5 drops of 0.5m dilute sulfuric acid to continue grinding, and grind the sample until the surface is wet.

[0033] (2) Transfer the ground sample in step (1) into a 50ml hydrothermal kettle, place it in a vacuum drying oven, and react at 180°C for 11 hours.

[0034] (3) Take out the carbon material precursor in step (2), transfer it into a quartz boat, place it in a tube furnace, and carbonize it in an atmosphere with a nitrogen flow rate of 100 ml / min. The heating rate is 2 °C / min, and the temperature is raised to 900 °C. , After 1.5 hours of heat preservation, cooling treatment.

[0035] (4) The sample obtained in step (3) was ground and pulverized, magnetically stirred with 0.5 m dilute hydrochloric acid for 6 hours, subjected to ultrasonic treatment for 2 hours and then filtered with suction, and the sample was dried in a blast dry...

Embodiment 3

[0038] (1) Take 1g of tannin, 1g of vanillin, and 4g of nano-calcium carbonate and mix them in a mortar. After fully grinding and mixing, add 4-5 drops of 0.5m dilute sulfuric acid to continue grinding, and grind the sample until the surface is wet.

[0039] (2) Transfer the ground sample in step (1) into a 50ml hydrothermal kettle, place it in a vacuum drying oven, and react at 180°C for 10 hours.

[0040] (3) Take out the carbon material precursor in step (2), transfer it into a quartz boat, place it in a tube furnace, and carbonize it in an atmosphere with a nitrogen flow rate of 100 ml / min. The heating rate is 2 °C / min, and the temperature is raised to 900 °C. , After 1.5 hours of heat preservation, cooling treatment.

[0041] (4) The sample obtained in step (3) was ground and pulverized, magnetically stirred with 0.5 m dilute hydrochloric acid for 6 hours, subjected to ultrasonic treatment for 2 hours and then filtered with suction, and the sample was dried in a blast dry...

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Abstract

The invention belongs to the field of preparation of porous materials, and mainly relates to preparation of solvent-free hydrothermal preparation method of a carbon material, which comprises the following steps: mixing tannic acid, vanillin and nano calcium carbonate, dropwise adding a small amount of dilute sulfuric acid, and grinding until the surface is wet; putting the ground sample into a vacuum drying oven for reaction; carbonizing the carbon material precursor in a nitrogen atmosphere, grinding and crushing the precursor, treating the precursor with diluted hydrochloric acid, drying theprecursor, treating with distilled water, and drying the precursor to obtain the carbon material prepared by the solvent-free hydrothermal method. According to the method, solid-solid mixing is carried out for hydrothermal reaction, wherein no solvent is added when the hydrothermal reaction is used for preparing the carbon material, and experiment risks are reduced, and a carbon material precursor is directly obtained after the experimental reaction. The prepared carbon material has good specific surface area and uniform pore size distribution, and can be further used for loading other metalmaterials.

Description

technical field [0001] The invention belongs to the field of porous material preparation, and mainly relates to the preparation of a solvent-free hydrothermal carbon material. [0002] technical background [0003] The preparation of carbon materials mostly adopts the solvent method, using ethylene glycol, isoacetone or absolute ethanol as a solvent, and reacting at high temperature. The solvent used in this type of method cannot be recovered, causing pollution; the process of collecting carbon materials after the experimental reaction is complicated and requires multiple centrifugal suction filtration; and such organic solvents are dangerous to operate at high temperatures. [0004] At present, most of the methods for preparing carbon materials by hydrothermal method require stirring and mixing an organic carbon source and a solvent and then placing them in a hydrothermal kettle, and acting at high temperature in a drying oven to generate carbon materials. [0005] However,...

Claims

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Application Information

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IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 胡勋周舒心
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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