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1. (WO2018220477) NITRURE DE CARBONE MÉSOPOREUX DE TYPE CAGE 3D À TENEUR ÉLEVÉE EN AZOTE À PARTIR DE PRÉCURSEURS DE DIAMINOGUANIDINE POUR LA CAPTURE ET LA CONVERSION DU CO2
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CLAIMS

A nitrogen rich three-dimensional graphitic mesoporous carbon nitride (gMCN) material having (i) a spherical morphology, (ii) a C3N4+ stoichiometry where the nitrogen to carbon (N/C) ratio from 1.45 to 1.6, and (iii) a monomodal pore distribution with an average pore diameter between 6.5 to 9.5 nm.

The material of claim 1, wherein the N/C ratio is 1.5.

The material of claim 1, wherein the gMCN is formed from templated diaminoguanidine, preferably 1,3-diaminoguanidine.

The material of claim 1, wherein the material has a BET surface area of 180 to 200 m2/g, preferably 190 to 198 m2/g.

The material of claim 1, wherein the material has a total pore volume of 0.4 - 0.7 cm3/g, preferably 0.5 cm3/g.

The material of claim 1, wherein the material has a CO2 adsorption capacity of 7.0 to 9.5 mmol/g at 273K and 30 bar.

The material of claims 1 to 6, wherein the material has an isosteric heat of adsorption of 10, 15, 20, 25, 30, 35 to 40, 45, 50, 55, 60, 65, 70, 75, 80 kJ/mol.

The material of claim 1, wherein the material is a negative replica of a FDU-12 silica template.

A method of synthesizing a three dimensional carbon nitride material formed from a diaminoguanidine precursor comprising:

(a) contacting a silica template with an aqueous diaminoguanidine precursor solution forming a templated reaction mixture;

(b) heating the templated reaction mixture to a temperature between 40 and 200 °C, preferably between 80 and 120 °C for 4 to 8 hours forming a first heated reaction mixture;

(c) heating the first heated reaction mixture to a temperature between 100 and 200 °C, preferably between 140 to 180 °C, preferable 160°C, for 4 to 8 hours forming a second heated reaction mixture;

(d) carbonizing the second heated reaction mixture by heating to about 300 to 500 °C, preferably 400 °C, for 4 to 6 hours forming a template/1, 3- diaminoguanidine-based carbon nitride product; and

(e) removing the template to form the nitrogen rich three-dimensional C3N4+ graphitic mesoporous carbon nitride (gMCN) material of any one of claims 1 to 8.

10. The method of claim 9, wherein the silica template is formed by:

(f) adding tetraethyl orthosilicate (TEOS) to a mixture of F-127 surfactant, potassium chloride (KC1), 1,3,5-trimethylbenzene, and hydrogen chloride (HQ) forming a template reaction mixture;

(g) incubating the template reaction mixture at a temperature of about 30 to 40 °C, preferably 35 °C for 1 to 4 hours;

(h) heating the template reaction mixture to 100 - 200 °C for 1 to 4 days forming a heated template reaction mixture;

(i) drying the heated template reaction mixture at 100 °C for 5 to 10 hours forming a dried template reaction mixture; and

(j) calcining the dried template reaction mixture at a temperature of 500 to 600 °C, preferably 540 °C, forming a FDU-12 silica template.

11. The method of claim 9, wherein the template reaction mixture is heated at a temperature of about 130 °C forming a FDU-12- 130 template.

12. The method of claim 9, wherein the template reaction mixture is heated at a temperature of about 150 °C forming a FDU-1-150 template.

13. The method of claim 9, further comprising crushing the second heated reaction mixture prior to the carbonizing.

14. The method of claim 9, further comprising bringing the second heated mixture to carbonization temperature using a ramping rate of 2 to 4 °C/min.

15. The method of claim 9, wherein carbonizing is performed under constant nitrogen flow.

16. The method of claim 9, wherein the first heated reaction mixture is incubated at a temperature of 130 °C

17. The method of claim 9, wherein the first heated reaction mixture is incubated at a temperature of 150 °C

18. The method of claim 9, wherein the template is removed by treating the template/diaminoguanidine-based carbon nitride product with hydrogen fluoride or an ethanol wash.

A CO2 capture process comprising contacting a nitrogen rich three-dimensional C3N4+ graphitic mesoporous carbon nitride (gMCN) of any one of claims 1 to 8, with a CO2 containing feed source, wherein CO2 is absorbed in or to gMCN.

The process of claim 19, further comprising incubating the CO2 absorbed gMCN under conversion conditions forming a CO2 conversion product.

The process of claim 20, wherein the CO2 conversion product comprises methanol.