Method for producing carbon aerogel from hydrogel precursor material by means of hydrothermal process

A precursor material, carbon aerogel technology, applied in the direction of airgel preparation, colloid chemistry, colloid chemistry, etc., can solve the problems of many steps in the preparation process, low overall yield, high precursor cost, etc., and achieve easy structure control , the effect of high overall yield

Active Publication Date: 2020-06-16
INST OF CHEM CHINESE ACAD OF SCI
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  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the above analysis, the embodiment of the present invention aims to provide a method for preparing carbon aerogels from hydrogel precursor materials through a hydrothermal process, in order to solve the following problems in the existing carbon aerogel preparation methods: 1) There are many steps in the preparation process, the cost of the precursor is

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  • Method for producing carbon aerogel from hydrogel precursor material by means of hydrothermal process
  • Method for producing carbon aerogel from hydrogel precursor material by means of hydrothermal process
  • Method for producing carbon aerogel from hydrogel precursor material by means of hydrothermal process

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Embodiment 1

[0055] Chitosan 1.6g, 36wt% concentrated hydrochloric acid 1.0g, water-soluble carbohydrate 20g and deionized water 77.4g form a uniform solution; then add 1.2g Tween-60 and 5.0g liquid paraffin, stir to form a uniformly dispersed system; dropwise 2.2g glutaraldehyde aqueous solution (50wt%), after stirring evenly, leave standstill to form hydrogel; The hydrogel is placed in the stainless steel reaction kettle that has polytetrafluoroethylene liner, left standstill reaction 4.0 hours at 180 ℃; Reaction After finishing, the primary carbonized product is cleaned to a neutral pH value by deionized water, and then by ethanol-n-butanol (V / V:2 / 1, 45g), n-butanol-n-hexane (V / V:3 / 1 , 50g) The system is subjected to solvent replacement in sequence, and the replaced primary carbonized product is vacuum-dried at room temperature until the quality remains unchanged; the dried primary carbonized product is further heat-treated at 800°C, and the heating rate of the process is 3.0°C / min. The...

Embodiment 2

[0059] Chitosan, 36wt% concentrated hydrochloric acid, glucose and deionized water form a uniform solution; then add Tween-60 and liquid paraffin, stir to form a uniformly dispersed system; dropwise add glutaraldehyde aqueous solution (50wt%) (concrete hydrogel composition The conditions are shown in Table 2), stirred evenly and then left to stand to form a hydrogel; the hydrogel was placed in a stainless steel reactor with a polytetrafluoroethylene lining, and was left to react at 180°C for 4.0 hours; after the reaction, the primary The carbonized product is cleaned by deionized water until the pH value is neutral, then by ethanol-n-butanol (V / V:2 / 1, 45g), n-butanol-n-hexane (V / V:3 / 1, 50g) The system was subjected to solvent replacement in sequence, and the replaced primary carbonized products were vacuum-dried at room temperature until the quality remained unchanged; the dried primary carbonized products were further heat-treated at 800 °C, the heating rate of the process was...

Embodiment 3

[0066] Chitosan 1.6g, 36wt% concentrated hydrochloric acid 1.0g, glucose 20g and deionized water 77.4g form a uniform solution; then add 1.2g Tween-60 and 5.0g liquid paraffin, stir to form a dispersed uniform system; Dialdehyde aqueous solution (50wt%), stirred evenly and left to stand to form a hydrogel; the hydrogel was placed in a stainless steel reaction kettle with a polytetrafluoroethylene lining, and was left to react at 180 ° C for 4.0 hours; after the reaction, the primary The carbonized product is cleaned by deionized water until the pH value is neutral, and then the solvent replacement is carried out in sequence by ethanol-n-butanol and n-butanol-n-hexane system (solvent replacement conditions are shown in Table 4), and the replaced primary carbonized product Vacuum drying at room temperature until the quality remains unchanged; the dried primary carbonized product is further heat-treated at 800°C, the heating rate of the process is 3.0°C / min, the nitrogen flow rate...

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Abstract

The invention relates to a method for preparing carbon aerogel from a hydrogel precursor material through a hydrothermal process, belongs to the field of new materials, and solves the problems of complex carbon preparation process and high cost due to adoption of supercritical drying in the prior art. The method comprises the following steps: step 1, acidifying chitosan with diluted hydrochloric acid, and forming a mixed solution with water-soluble carbohydrates; step 2, adding a polysorbate nonionic surfactant and liquid paraffin, and then adding glutaraldehyde to form hydrogel; step 3, placing the hydrogel in a reaction kettle, and carrying out a hydrothermal reaction, to obtain a primary carbonization product; step 4, cleaning the primary carbonization product and replacing the primarycarbonization product with a two-stage solvent; and step 5, carrying out further heat treatment on the primary carbonization product, characterizing the microstructure of the primary carbonization product by using a scanning electron microscope, and determining the pore property of the sample by nitrogen adsorption. The carbon aerogel structure is generated in one step by utilizing low-cost raw materials; normal-pressure drying of the carbon aerogel structure is achieved through two-stage solvent replacement.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a method for preparing carbon airgel from a hydrogel precursor material through a hydrothermal process. Background technique [0002] Kistler first proposed the concept of airgel in 1932, which refers to a solid structure that does not collapse after the liquid in the gel is replaced by gas. Silica structure is the most researched airgel, which is relatively mature. In 2003, Aspen Aerogels and Cabot Aerogels have begun mass production of silica airgel particles and molding materials. [0003] Carbon aerogels are a relatively special class of materials, which usually require an organic high-resolution airgel as a precursor and are obtained through carbonization. The precursor materials commonly used in carbon airgel are: resorcinol formaldehyde airgel (RF), melamine formaldehyde airgel (MF), phenolic airgel (PF), polyacrylonitrile and polyurethane system . The application...

Claims

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Application Information

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IPC IPC(8): C01B32/05B01J13/00
CPCB01J13/0091C01B32/05
Inventor 李峰波袁国卿宋延林
Owner INST OF CHEM CHINESE ACAD OF SCI
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