Method of synthesis of CMK-3-type carbon replica

Patent metadata

Field	Value
Publication number	US-9302252-B2
Application number	US-201314374566-A
Country	US
Kind code	B2
Filing date	Feb 8, 2013
Priority date	Feb 14, 2012
Publication date	Apr 5, 2016
Grant date	Apr 5, 2016

Abstract

The method of obtaining the CMK-3-type carbon replica, consisting of the introduction of SBA-15-type molecular sieve to a mixture of furfuryl alcohol and a solvent, the subsequent polycondensation of furfuryl alcohol, carbonization of the prepared, composite and removal of the hard template, according to the invention, is characterized in that the reaction of furfuryl alcohol polycondensation is carried out by the precipitation method in a slurry containing SBA-15 silica sieve, water, furfuryl alcohol and concentrated solution of hydrochloric acid in mass ratios, respectively, in the range from 1.00:32.33:1.00:6.65 to 1.00:30.83:2.50:16.64, whereas the ratio of the total mass of furfuryl alcohol and water to the mass of SBA-15 as well as the mass ratio of the concentrated HCl solution to the mass of furfuryl alcohol are kept at the constant value every time.

First claim

The invention claimed is:

1. The method of obtaining the CMK-3-type carbon replica, consisting of the introduction of SBA-15-type silica mesoporous sieve to a mixture of furfuryl alcohol and a solvent, the subsequent polycondensation of furfuryl alcohol, carbonization of the prepared composite and removal of hard template (SIO 2 ), wherein the reaction of furfuryl alcohol polycondensation is carried out by the precipitation method in a slurry containing SBA-15 silica sieve, water, furfuryl alcohol and concentrated solution of hydrochloric acid in mass ratios, respectively, in the range from 1.00:32.33:1.00:6.65 to 1.00:30.83:2.50:16.64, whereas the ratio of the total mass of furfuryl alcohol and water to the mass of SBA-15 as well as the mass ratio of the concentrated HCl solution to the mass of furfuryl alcohol are kept at the constant value for each synthesis.

2. The method according to claim 1 , wherein said the polycondensation process is carried out at a temperature from the range of 30-100° C.

3. The method according to claim 1 , wherein said polycondensation process is carried out for a time not less than 1 hour.

4. The method of obtaining the CMK-3-type carbon replica comprising:
a) introducing SBA-15-type silica mesoporous sieve to a mixture of furfuryl alcohol and a solvent;
b) subsequent to a) carrying out a reaction of furfuryl alcohol polycondensation by a precipitation method in a slurry containing SBA-15 silica sieve, water, furfuryl alcohol and concentrated solution of hydrochloric acid in mass ratios, respectively, in the range from 1.00:32.33:1.00:6.65 to 1.00:30.83:2.50:16.64, wherein the ratio of the total mass of furfuryl alcohol and water to the mass of SBA-15 as well as the mass ratio of the concentrated HCl solution to the mass of furfuryl alcohol are kept at a constant value for each synthesis;
c) carbonizing the prepared composite from b); and
d) removing a hard template (SIO 2 ) from the carbonized composite.

5. The method according to claim 4 including prior to c), isolating PFA/SBA-15 precipitate that resulted from b).

6. The method according to claim 4 including prior to a), drying the SBA-15-type silica mesoporous at 150° C. for 24 hours.

7. The method according to claim 4 , wherein c) is performed in a flow of inert gas.

8. The method according to claim 4 , wherein d) includes treating the carbonized composite with a solution of hydrofluoric acid.

9. The method according to claim 4 , wherein the polycondensation process is carried out at a temperature from the range of 30-100° C.

10. The method according to claim 4 , wherein the polycondensation process is carried out for a time not less than 1 hour.

11. The method according to claim 4 , wherein a) includes stirring the obtained slurry of SBA-15-type silica mesoporous sieve and the furfuryl alcohol and solvent mixture at 400 rpm at room temperature for 30 minutes.

Assignees

• Univ Jagiellonski

Inventors

• Kustrowski Piotr
• Janus Rafal
• Niebrzydowska Paula

Classifications

• B01J2235/15

  X-ray diffraction · CPC title

• B01J20/20

  comprising free carbon; comprising carbon obtained by carbonising processes · CPC title

• B01J21/18

  Carbon · CPC title

• B01J20/3057

  Use of a templating or imprinting material (molecularly imprinted polymers B01J20/268); filling pores of a substrate or matrix followed by the removal of the substrate or matrix · CPC title

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title