Carbonate-promoted carboxylation at high rates
A method for synthesizing furan-2, 5-dicarboxylate (FDCA 2− ) is provided. Furan-2-carboxylate is provided with an inorganic base in the form of an inorganic base salt, wherein the furan-2-carboxylate and the inorganic base salt form a mixture. A CO 2 gas is provided to the mixture. The mixture is heated to a temperature to at least partially melt the mixture, wherein the heating of the mixture causes the synthesizing of a M x FDCA solid, wherein M x FDCA denotes a salt comprising furan-2,5-dicarboxylate (FDCA 2− ) and cation M + and/or M 2+ , where x is a number between 1 and 2, inclusive. The mixture containing furan-2-carboxylate is mechanically agitated, wherein the mechanically agitating breaks up the M x FDCA solid.
1. A method for synthesizing furan-2, 5-dicarboxylate (FDCA 2−) , comprising:
providing furan-2-carboxylate;
providing an inorganic base in a form of an inorganic base salt, wherein the furan-2-carboxylate and the inorganic base salt form a mixture;
providing a CO 2 gas to the mixture;
heating the mixture to a temperature to at least partially melt the mixture, wherein the heating of the mixture causes the synthesizing of a M x FDCA solid, wherein M x FDCA denotes a salt comprising furan-2,5-dicarboxylate (FDCA 2−) and cation M + or M 2+ , where x is a number between 1 and 2, inclusive; and
mechanically agitating the mixture containing furan-2-carboxylate, wherein the mechanically agitating breaks up the M x FDCA solid.
2. The method, as recited in claim 1 , wherein the inorganic base salt is a CO 3 2− salt.
3. The method, as recited in claim 2 , wherein cation M + is an alkali cation and cation M 2+ is an alkaline earth cation.
4. The method, as recited in claim 2 , wherein M + is a Cs + cation.
5. The method, as recited in claim 1 wherein the mechanically agitating is performed using an impellor, wherein a speed of rotation of the impellor and geometry of the impellor allow the impeller to break up the M x FDCA solid.
6. The method, as recited in claim 1 wherein the mechanically agitating is performed in an extruder using one or more screws to break up the M x FDCA solid.
7. The method, as recited in claim 1 wherein the mechanically agitating is performed in a ball mill.
8. The method, as recited in claim 1 wherein CO 2 is flowed through a reactor for agitating the mixture.
9. The method, as recited in claim 1 , wherein the mixture is substantially catalyst free.
10. The method, as recited in claim 1 , wherein the mixture is substantially free of zinc compounds, cadmium compounds, mercury compounds, and iron compounds.
11. The method, as recited in claim 1 , wherein heating the mixture is substantially free of metal containing catalyst.
12. The method, as recited in claim 1 , wherein the inorganic base salt and CO 2 gas form a CO 3 2− salt.
13. The method, as recited in claim 1 , wherein the providing furan-2-carboxylate provides furan-2-carboxylate in a solution and wherein the providing the inorganic base provides the inorganic base in a solution, wherein the mixture is a solution with a solvent, further comprising removing the solvent of the solution.
14. A method for synthesizing furan-2, 5-dicarboxylate (FDCA 2−) , comprising:
providing furan-2-carboxylate;
providing an inorganic base in a form of an inorganic base salt, wherein the furan-2-carboxylate and the inorganic base salt form a mixture;
providing a CO 2 gas to the mixture;
heating the mixture to a temperature to at least partially melt the mixture, wherein the heating of the mixture causes the synthesizing of a M x FDCA solid, wherein M x FDCA denotes a salt comprising furan-2,5-dicarboxylate (FDCA 2−) and cation M + or M 2+ , where x is a number between 1 and 2, inclusive; and
cooling the mixture to solidify the mixture to form a solid mixture;
reducing particle sizes of the solid mixture; and
reheating the mixture while providing a CO 2 gas to partially melt the mixture.
15. The method as cited in claim 14 , wherein the cooling the mixture to solidify the mixture reduces sizes of the solid mixture.
16. The method, as recited in claim 14 , wherein the inorganic base salt is a CO 3 2− salt.
17. The method, as recited in claim 14 , wherein M + is an alkali cation or mixture of alkali cations.
18. The method, as recited in claim 14 , wherein M + is a Cs + cation.
19. The method, as recited in claim 14 , wherein the heating of the mixture is substantially catalyst free.
20. The method, as recited in claim 14 , wherein the heating of the mixture is substantially free of zinc compounds, cadmium compounds, mercury compounds, and iron compounds.