Synthesis of porous graphitic carbon membranes

Patent metadata

Field	Value
Publication number	US-12138594-B2
Application number	US-202017609515-A
Country	US
Kind code	B2
Filing date	May 10, 2020
Priority date	May 10, 2019
Publication date	Nov 12, 2024
Grant date	Nov 12, 2024

Abstract

Methods for preparation of a carbon membrane include providing a solution comprising a diacetyl biphenyl monomer and an alkylsulfonic acid. The solution is treated under such conditions that an aldol condensation reaction occurs so as to produce a porous polymer network. The porous polymer network is treated under such conditions that a Scholl reaction occurs.

First claim

The invention is claimed as follows:

1. A method for preparation of a carbon membrane, the method comprising:
providing a first solution comprising a diacetyl biphenyl monomer and an alkylsulfonic acid;
treating the first solution under such conditions that an aldol condensation reaction occurs to produce a porous polymer network;
treating the porous polymer network under such conditions that a Scholl reaction occurs;
synthesizing a porous carbon precursor; and
wherein the synthesizing of the porous carbon precursor comprises:
heating the first solution to a temperature between 100° C. and 200° C.;
cooling the first solution; and
extracting the porous carbon precursor;

synthesizing a porous graphitic carbon;
the synthesizing of the porous graphitic carbon comprises:
providing a suspension comprising the porous carbon precursor;
bubbling the suspension with N 2 ;
adding to the suspension a mixture comprising FeCl 3 and MeNO 2 dropwise; and
stirring the suspension.

2. The method of claim 1 , wherein the first solution comprises a plurality of diacetyl biphenyl monomers.

3. The method of claim 1 , wherein the aldol condensation reaction comprises an aldol triple condensation reaction.

4. The method of claim 1 , wherein the alkylsulfonic acid comprises methanesulfonic acid (MSA).

5. The method of claim 1 , wherein the porous polymer network comprises a conjugated porous polymer network.

6. The method of claim 1 , wherein the diacetyl biphenyl monomer comprises 2,2′-diacetyl-1,1′-biphenyl.

7. The method of claim 1 further comprising synthesizing the diacetyl biphenyl monomer.

8. The method of claim 7 , wherein the synthesizing of the diacetyl biphenyl monomer comprising
providing a second solution comprising 2′-Iodoacetophenone, copper powder, and CuTc;
heating the second solution; and
cooling the second solution.

9. The method of claim 8 , wherein the heating of the second solution comprises heating the second solution to a temperature below 100° C. under N 2 .

10. The method of claim 8 , wherein the heating of the second solution comprises heating the second solution to a temperature up to 70° C.

11. The method of claim 8 , wherein the heating of the second solution comprises heating the second solution for about 24 hours.

12. The method of claim 8 , wherein the cooling of the second solution comprises cooling the second solution to room temperature.

13. The method of claim 1 comprising providing the first solution between two pieces of glass; and heating the two pieces of glass to the temperature between 100° C. and 200° C.

14. The method of claim 13 , wherein the heating of the two pieces of glass comprises heating the two pieces of glass at about 150° C. for about 24 hours.

15. A method for preparation of a carbon membrane, the method comprising:
providing a first solution comprising a diacetyl biphenyl monomer and an alkylsulfonic acid;
treating the first solution under such conditions that an aldol condensation reaction occurs to produce a porous polymer network;
treating the porous polymer network under such conditions that a Scholl reaction occurs;
synthesizing a porous carbon precursor; and
wherein the synthesizing of the porous carbon precursor comprises:
heating the first solution to a temperature between 100° C. and 200° C.;
cooling the first solution; and
extracting the porous carbon precursor;

synthesizing a porous graphitic carbon;
the synthesizing of the porous graphitic carbon comprises:
providing a suspension comprising the porous carbon precursor;
bubbling the suspension with N 2 ;
adding to the suspension a mixture comprising FeCl 3 and MeNO 2 dropwise; and
stirring the suspension; and

wherein the diacetyl biphenyl monomer allows for the preparation of conductive, graphitic carbon materials.

16. The method of claim 15 , wherein the heating of the first solution comprises heating the first solution to the temperature at about 150° C. for about 24 hours.

17. The method of claim 1 , wherein the heating of the first solution comprises heating the first solution to the temperature at about 150° C. for about 24 hours.

Assignees

• Qatar Found Education Science & Community Dev
• Total E&P Golfe Ltd

Inventors

• Fang Lei
• Che Sai
• Wang Chenxu
• Al-Hashimi Mohammed
• Banerjee Sarbajit

Classifications

• B01D71/0211

  Graphene or derivates thereof · CPC title

• B01D2323/081

  Heating · CPC title

• B01D67/0058

  by selective elimination of components, e.g. by leaching · CPC title

• B01D67/0044

  by chemical reaction · CPC title

• C08G6/00 Primary

  Condensation polymers of aldehydes or ketones only · CPC title