Method for producing a macroporous and mesoporous geopolymer, with controlled porosity

Patent metadata

Field	Value
Publication number	US-10322966-B2
Application number	US-201515129037-A
Country	US
Kind code	B2
Filing date	Mar 27, 2015
Priority date	Mar 27, 2014
Publication date	Jun 18, 2019
Grant date	Jun 18, 2019

Abstract

The present invention relates to a method for preparing a macroporous and mesoporous geopolymer and especially a geopolymer foam, comprising the following successive steps (1) preparing a composite material comprising a geopolymer matrix and an organic liquid; then (2) eliminating said organic liquid by a treatment selected from the group consisting of heat treatment, oxidation treatment, photodegradation treatment and extraction using a supercritical fluid or ultrasounds.

First claim

The invention claimed is:

1. A method for preparing a macroporous and mesoporous geopolymer comprising the successive steps consisting of:
1) preparing a composite material comprising a geopolymer matrix and an organic liquid; and then
2) removing said organic liquid by a treatment selected from the group consisting of at least one of a heat treatment, oxidation treatment, photodegradation treatment and an extraction via a supercritical fluid or ultrasounds,
wherein said step (1) comprises the following sub-steps:
a) preparing an activation solution comprising said organic liquid,
b) adding to the solution obtained in step (a) at least one alumino-silicate source,
c) subjecting the mixture obtained in step (b) to conditions allowing hardening of the geopolymer.

2. The method according to claim 1 , wherein the composite material prepared during said step (1) appears as a geopolymer or a geopolymeric matrix in which beads of organic liquid and microbeads and/or nanobeads of organic liquid are coated.

3. The method according to claim 1 , wherein said organic liquid comprises at most 50% of triglycerides by mass based on the total dry mass of said organic liquid.

4. The method according to claim 1 , wherein said organic liquid is an unsaponifiable organic liquid.

5. The method according to claim 1 , wherein said organic liquid comprises a thermally insulating oil.

6. The method according to claim 1 , wherein said organic liquid comprises at least one element selected from the group consisting of a naphthenic oil; an aliphatic hydrocarbon; an unsaturated linear synthetic hydrocarbon; an aromatic hydrocarbon; a chlorinated linear hydrocarbon; a chlorinated aromatic hydrocarbon; a chlorinated-fluorinated linear hydrocarbon; an ethylenic aromatic hydrocarbon; a chlorinated solvent; an oxygenated solvent; an alkyl phosphate; an alkyl chloride and a liquid silicone.

7. The method according to claim 1 , wherein said organic liquid comprises at least one element selected from the group consisting of commercial scintillator liquid, motor oil, oil for transformers, benzene, alkylbenzene, alkylnaphthalene, alkylbiphenyl, toluene, xylene, ethylbenzene, kerosene, hexane, cyclohexane, octane, ethylcyclohexane, dodecane, eicosane, phenol, dichloromethane, trichloroethane, dichlorobenzene, trichloroethylene, perchlorethylene, trichlorobenzene, polychlorobiphenyl, trichloro-trifluoroethane, alkyldiarylethylene, 2-octanone, 4-dodecanone, tributyl phosphate (TBP), tetrahydrofuran (THF), diethyl ether, polydimethylsiloxane and polydiphenylsiloxane.

8. The method according to claim 1 , wherein surfactant(s) is(are) added (α) to said activation solution prior to the addition of said organic liquid, (β) to said organic liquid prior to its addition in said activation solution or (γ) to said activation solution into which the organic liquid has already been added.

9. The method according to claim 1 , wherein in addition to the alumino-silicate source, sand, granulate and/or fines are added to the activation solution during said sub-step (b).

10. The method according to claim 1 , wherein said heat treatment consists of subjecting the composite material of step (1) to a temperature above 200° C.

11. The method according to claim 1 , wherein said oxidation treatment is either a plasma treatment or an ozone treatment.

12. The method according to claim 1 , wherein said supercritical fluid is selected from the group consisting of at least one of supercritical carbon dioxide (CO 2 ), supercritical nitrogen monoxide (N 2 O), supercritical chlorodifluoromethane, supercritical trifluoromethane, supercritical methanol, supercritical hexane and supercritical water.

13. The method according to claim 3 , wherein said organic liquid comprises at most 40% of triglycerides by mass based on the total dry mass of said organic liquid.

14. The method according to claim 3 , wherein said organic liquid comprises at most 30% of triglycerides by mass based on the total dry mass of said organic liquid.

15. The method according to claim 3 , wherein said organic liquid comprises at most 20% of triglycerides by mass based on the total dry mass of said organic liquid.

16. The method according to claim 3 , wherein said organic liquid comprises at most 10% of triglycerides by mass based on the total dry mass of said organic liquid.

17. The method according to claim 1 , wherein said organic liquid is a thermally insulating oil.

18. The method according to claim 1 , wherein said organic liquid is at least one element selected from the group consisting of a naphthenic oil; an aliphatic hydrocarbon; an unsaturated linear synthetic hydrocarbon; an aromatic hydrocarbon; a chlorinated linear hydrocarbon; a chlorinated aromatic hydrocarbon; a chlorinated-fluorinated linear hydrocarbon; an ethylenic aromatic hydrocarbon; a chlorinated solvent; an oxygenated solvent; an alkyl phosphate; an alkyl chloride and a liquid silicone.

19. The method according to claim 1 , wherein said organic liquid is at least one element selected from the group consisting of commercial scintillator liquid, motor oil, oil for transformers, benzene, alkylbenzene, alkylnaphthalene, alkylbiphenyl, toluene, xylene, ethylbenzene, kerosene, hexane, cyclohexane, octane, ethylcyclohexane, dodecane, eicosane, phenol, dichloromethane, trichloroethane, dichlorobenzene, trichloroethylene, perchlorethylene, trichlorobenzene, polychlorobiphenyl, trichloro-trifluoroethane, alkyldiarylethylene, 2-octanone, 4-dodecanone, tributyl phosphate (TBP), tetrahydrofuran (THF), diethyl ether, polydimethylsiloxane and polydiphenylsiloxane.

20. The method according to claim 10 , wherein said heat treatment consists of subjecting the composite material of step (1) to a temperature between 300° C. and 1,000° C.

21. The method according to claim 10 , wherein said heat treatment consists of subjecting the composite material of step (1) to a temperature between 400° C. and 800° C.

22. The method according to claim 1 , wherein said organic liquid comprises at least one element selected from the group consisting of an aromatic synthetic hydrocarbon, an alcohol, a ketone, a glycol ether and an ether oxide.

23. The method according to claim 1 , wherein said organic liquid is at least one element selected from the group consisting of an aromatic synthetic hydrocarbon, an alcohol, a ketone, a glycol ether and an ether oxide.

Assignees

• Commissariat Energie Atomique

Inventors

• Lambertin David
• Poulesquen Arnaud
• Frizon Fabien
• Rooses Adrien
• Goettmann Frederic

Classifications

• C04B28/006

  containing mineral polymers, e.g. geopolymers of the Davidovits type · CPC title

• C04B38/0645

  Burnable, meltable, sublimable materials · CPC title

• C04B12/005 Primary

  Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates · CPC title

• C04B40/0028

  Aspects relating to the mixing step of the mortar preparation · CPC title

• C04B38/0064

  Multimodal pore size distribution · CPC title