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Method for synthesis of furfural-phenolic aldehyde based charcoal aerogel

A synthesis method, a technology of phenolic-based carbon, applied in chemical instruments and methods, bulk chemical production, other chemical processes, etc., can solve the problems of poor structural adjustability, macroporous aerogel, and high price, and achieve adjustable The effect of wide range, good structure controllability and low product cost

Inactive Publication Date: 2003-03-12
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because resorcinol is expensive, its industrial application is limited
U.S. Patent No. 5,476,878 discloses a method for preparing organic aerogels and its cracked products—carbon aerogels using novolac resins and furfural under organic solvents and acidic conditions, but this method has the following disadvantages: the first, the resin used It is a novolac phenolic resin with high molecular weight and poor structure adjustability, and the prepared airgel has more macropores
Second, the solvent used is n-propanol, the price is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Make a solution according to water-soluble phenolic resin No. 2 (see note) 100g (dry base), 100g furfural, and 0.25Kg water, adjust the pH to 8.0 with catalyst-sodium carbonate, put it in a container and polymerize at a constant temperature of 70°C 24 hours; replace the water in the gel with 1 times acetone, once a day, a total of 3 replacements; put the ketone gel in a 5-liter autoclave and fill it with acetone, raise the temperature to 250 ° C, and keep the autoclave during the heating process The pressure is 8.2MPa, keep the temperature constant for 3 hours, then lower the pressure and then lower the temperature; put the obtained organic airgel in a cracking furnace, raise the temperature to 850°C at 5°C / min under the protection of nitrogen and keep the temperature constant for 3 hours to obtain carbon airgel . The BET specific surface of the carbon airgel is 1200m 2 / g, pore volume 1.5cm 3 / g.

Embodiment 2

[0021] Water-soluble phenolic resin No. 1 (see Note) 160g (dry basis), furfural 40g, water 0.75Kg, catalyst potassium hydroxide, pH 7.2, polymerization temperature 95 °C, time 180 hours, use methanol to replace coagulation The water in the glue was dried with methanol as drying medium at 275° C. and 6 MPa for 1.5 hours to obtain an organic aerogel, and under the protection of argon, it was cracked at 1800° C. for 15 minutes to obtain a carbon aerogel, and the rest were the same as in Example 1. The resulting carbon airgel BET specific surface is 558m 2 / g, the pore volume is 2.0cm 3 / g.

Embodiment 3

[0023] Water-soluble phenolic resin No. 3 (see note) 40g (dry basis), furfural is 160g, water is 6.5Kg, catalyst calcium hydroxide, pH is 6.5, polymerization temperature is 40°C, time is 360 hours, replacement solvent is methanol, Use methanol as drying medium, dry at 300° C. and 12 MPa for 0.1 hour to obtain an organic airgel, and under nitrogen protection, crack at 450° C. for 5 hours to obtain a carbon aerogel, and the rest are the same as in Example 1. The resulting carbon airgel has a BET specific surface of 754m 2 / g, the pore volume is 2.5cm 3 / g.

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Abstract

A process for synthesizing a furfural-phenolic aldehyde based carbon aerogel includes polymerizing furfural with phenolic resin in aqueous solution under catalysis of alkali to obtain sol and wet gel, displacing the water in wet gel by organic solvent, drying the gel in supercritical solvent, and cracking the dried gel in inert gas. The resultant carbon aerogel is a 3D space unit (3-200 nm) with a core of glass carbon particle (10 nm). Its advantages are simple regulatable range and low cost.

Description

Technical field: [0001] The invention relates to a method for preparing carbon airgel by using a sol-gel method, in particular to a synthesis method of furfural-phenolic carbon airgel. Background technique: [0002] When the size of the substance is on the nanometer scale (1 to 100 nanometers), its properties are significantly different from the properties of the macro and micro scales, that is, a sudden change occurs, showing surface effects, quantum confinement effects, small size effects, and macroscopic quantum tunneling effects and other physical and chemical properties. The sol-gel method is an important method for preparing nanomaterials, and has been applied to the preparation of many nanomaterials, such as silica aerogels, zirconia aerogels, etc. Carbon aerogels can be widely used in supercapacitor electrodes, chromatographic fillers, drinking water purification, and thermal insulation materials in high-temperature applications. Document (R.W.Pekala, Organic aerog...

Claims

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Application Information

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IPC IPC(8): B01J20/22C08J9/28
CPCY02P20/54
Inventor 凌立成张睿李开喜吕春祥朱星明
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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