PROCESS FOR PRODUCING POROUS MATERIALS

Abstract

The present invention relates to a process for preparing a porous material, at least comprising the steps of providing a mixture (I) comprising a composition (A) comprising components suitable to form an organic gel and a solvent (B), reacting the components in the composition (A) in the presence of the solvent (B) to form a gel, and drying of the gel obtained in step b). According to the present invention, the composition (A) comprises a catalyst system (CS) comprising a component (C1) selected from the group consisting of alkali metal and earth alkali metal salts of a saturated or unsaturated carboxylic acid and a component (C2) selected from the group consisting of ammonium salts of a saturated or unsaturated carboxylic acid and no carboxylic acid is used as a component of the catalyst system. The invention further relates to the porous materials which can be obtained in this way and the use of the porous materials as thermal insulation material and in vacuum insulation panels, in particular in interior or exterior thermal insulation systems as well as in water tank or ice maker insulation systems.

Claims

1. A process for preparing a porous material, the process comprising: reacting a composition (A) in the presence of a solvent (B), to form a gel; and drying the gel; wherein the composition (A) comprises a catalyst system (CS) comprising: a component (C1) selected from the group consisting of an alkali metal salt of a saturated carboxylic acid, an alkali metal salt of an unsaturated carboxylic acid, an alkaline earth metal salt of a saturated carboxylic acid, an alkaline earth metal salt of an unsaturated carboxylic acid, and mixtures thereof; and a component (C2) selected from the group consisting of an ammonium salt of a saturated carboxylic acid and an ammonium salt of an unsaturated carboxylic acid, and mixtures thereof, and wherein no carboxylic acid is present as a component of the catalyst system (CS).

2. The process of claim 1, wherein the catalyst component (C1) is selected from the group consisting of an alkali metal salt of a saturated carboxylic acid having 1 to 20 carbon atoms, an alkali metal salt of an unsaturated carboxylic acid having 1 to 20 carbon atoms, an alkaline earth metal salt of a saturated carboxylic acid having 1 to 20 carbon atoms, an alkaline earth metal salt of an unsaturated carboxylic acid having 1 to 20 carbon atoms, and mixtures thereof.

3. The process of claim 1, wherein the catalyst component (C2) is selected from the group consisting of an ammonium salt of a saturated carboxylic acid having 1 to 20 carbon atoms, an ammonium salt of an unsaturated carboxylic acid having 1 to 20 carbon atoms, and mixtures thereof.

4. The process of claim 1, wherein the catalyst component (C1) is selected from the group consisting of a potassium salt of a saturated carboxylic acid having 1 to 20 carbon atoms and a potassium salt of an unsaturated carboxylic acid having 1 to 20 carbon atoms, and wherein the catalyst component (C2) is selected from the group consisting of an ammonium salt of a saturated carboxylic acid having 1 to 20 carbon atoms, an ammonium salt of an unsaturated carboxylic acid having 1 to 20 carbon atoms, and mixtures thereof.

5. The process of claim 1, wherein the catalyst system (CS) is present in the composition (A) in an amount in a range of 0.1 to 30% by weight, based on the total weight of the composition (A).

6. The process of claim 1, wherein the catalyst system (CS) comprises catalyst components (C1) and (C2) in a ratio in a range of 1:20 to 20:1.

7. The process of claim 1, wherein the composition (A) further comprises a monool (am).

8. The process of claim 1, wherein the composition (A) further comprises a polyfunctional isocyanate as a component (a1).

9. The process of claim 1, wherein the composition (A) further comprises a polyfunctional isocyanate as a component (a1), and an aromatic amine as a component (a2), optionally water as a component (a3), and optionally a further catalyst as a component (a4).

10. The process of claim 9, wherein the aromatic amine (a2) is a polyfunctional aromatic amine.

11. The process of claim 9, wherein the aromatic amine (a2) has a formula (I): ##STR00006## wherein: R.sup.1 and R.sup.2 are each independently selected from the group consisting of hydrogen, a linear alkyl group having 1 to 6 carbon atoms, and a branched alkyl group having 1 to 6 carbon atoms; Q.sup.1 to Q.sup.5 and Q.sup.1 to Q.sup.5 are each independently selected from the group consisting of hydrogen, a primary amino group, a linear alkyl group having 1 to 12 carbon atoms, and a branched alkyl group having from 1 to 12 carbon atoms; and wherein the alkyl group of R.sup.1, R.sup.2, Q.sup.1 to Q.sup.5, and Q.sup.1 to Q.sup.5 can bear one or more further functional groups; with the proviso that at least one of Q.sup.1, Q.sup.3 and Q.sup.5 is a primary amino group, and at least one of Q.sup.1, Q.sup.3 and Q.sup.5 is a primary amino group.

12. The process of claim 1, wherein composition (A) comprises: (a0) 0.1 to 30% by weight of the catalyst system (CS); (a1) 25 to 94.9% by weight of at least one polyfunctional isocyanate; (a2) 0.1 to 30% by weight of at least one polyfunctional aromatic amine having a formula (I): ##STR00007## wherein: R.sup.1 and R.sup.2 are each independently selected from the group consisting of hydrogen, a linear alkyl group having 1 to 6 carbon atoms, and a branched alkyl group having 1 to 6 carbon atoms; Q.sup.1 to Q.sup.5 and to Q.sup.5 are each independently selected from the group consisting of hydrogen, a primary amino group, a linear alkyl group having 1 to 12 carbon atoms, and a branched alkyl group having from 1 to 12 carbon atoms; wherein the alkyl group of R.sup.1, R.sup.2, Q.sup.1 to Q.sup.5, and Q.sup.1 to Q.sup.5 can bear one or more further functional groups; with the proviso that at least one of Q.sup.1, Q.sup.3 and Q.sup.5 is a primary amino group, and at least one of Q.sup.1, Q.sup.3 and Q.sup.5 is a primary amino group; (a3) 0 to 15% by weight of water; and (a4) 0 to 29.9% by weight of at least one further catalyst; in each case based on a total weight of the components (a0) to (a4), where the % by weight of the components (a0) to (a4) adds up to 100% by weight, and wherein the sum of the components (a0) and (a4) is in a range of 0.1 to 30% by weight based on a total weight of the components (a0) to (a4).

13. The process of claim 9, wherein the amine component (a2) comprises a compound selected from the group consisting of 3,3,5,5-tetraalkyl-4,4-diaminodiphenylmethane, 3,3,5,5-tetraalkyl-2,2-diaminodiphenylmethane and 3,3,5,5-tetraalkyl-2,4-diaminodiphenylmethane, where the alkyl groups in the 3,3,5 and 5 positions can be identical or different and are selected independently from among linear or branched alkyl groups which have from 1 to 12 carbon atoms and can bear further functional groups.

14. The process of claim 9, wherein component (a0) or component (a4) or component (a0) and component (a4) catalyze a trimerization to form isocyanurate groups.

15. The process of claim 9, wherein component (a4) comprises a tertiary amino group.

16. The process of claim 1, wherein no water (a3) is present.

17. The process of claim 1, wherein the drying converts a liquid in the gel into the gaseous state at a temperature and a pressure below a critical temperature and a critical pressure of the liquid in the gel.

18. The process of claim 1, wherein the drying is carried out under supercritical conditions.

19. A porous material obtained by the process of claim 1.

20. A thermal insulation material, a vacuum insulation panel, an exterior or interior thermal insulation system, a water tank or ice maker thermal insulation system, or an insulation of thermal bridges, comprising: the porous material of claim 19.

21-23. (canceled)

Description

EXAMPLES

1. Methods

[0277] 1.1 Determination of Thermal Conductivity [0278] The thermal conductivity was measured according to DIN EN 12667 with a heat flow meter from Hesto (Lambda Control A50).

[0279] 1.2 Solvent Extraction with Supercritical Carbon Dioxide [0280] One or several gel monoliths were placed onto sample trays in an autoclave of 25 l volume. Subsequent to filling with supercritical carbon dioxide (scCO.sub.2), the gelation solvent was removed (drying) by flowing scCO.sub.2 through the autoclave for 24 h (20 kg/h). Process pressure was kept between 120 and 130 bar and process temperature at 55 C. in order to maintain carbon dioxide in a supercritical state. At the end of the process, the pressure was reduced to normal atmospheric pressure in a controlled manner while maintaining the system at a temperature of 55 C. The autoclave was opened, and the obtained porous monoliths were removed.

2. Materials

[0281] Component a1: oligomeric MDI (Lupranat M200) having an NCO content of 30.9 g per 100 g accordance with ASTM D-5155-96 A, a functionality in the region of three and a viscosity of 2200 mPa.Math.s at 25 C. in accordance with DIN 53018 (hereafter M200) [0282] Component a2: 3,3,5,5-Tetraethyl-4,4diaminodiphenylmethane (hereinafter MDEA) [0283] Catalysts a0: Potassium acetate dissolved in monoethylene glycol (5% by weight, 10% by weight, 15% by weight, 20% by weight) [0284] Ammonium acetate dissolved in monoethylene glycol 10% by weight, 20% by weight, 30% by weight) [0285] Potassium sorbate dissolved in monoethylene glycol (5% by weight, 10% by weight, 15% by weight) [0286] Triethylammonium sorbate dissolved in monoethylene glycol (90% by weight) [0287] Dabco K15 (potassium ethylhexanoate dissolved in diethylene glycol (85% by weight) [0288] Ammonium ethylhexanoate dissolved in monoethylene glycol (30% by weight, 50% by weight, 70% by weight, 80% by weight) [0289] Triethylammonium ethylhexanoate dissolved in monoethylene glycol (30% by weight, 50% by weight, 70% by weight, 90% by weight) 2,2,6,6-Tetramethylpiperidinium ethylhexanoate dissolved in monoethylene glycol (30% by weight, 50% by weight, 70% by weight) [0290] Dimethyluronium ethylhexanoate dissolved in monoethylene glycol (30% by weight, 50% by weight, 70% by weight) [0291] Flame retardant: Exolit OP 560 [0292] Additive: Graphite

3. Examples

[0293] Thermal conductivity values for all examples are shown in Table 1. Furthermore, data regarding the compressive strength and density are included for several examples.

3.1 Example 1 (Comparative)

[0294] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g Dabco K15 and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.2 Example 2 (Comparative)

[0295] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g Ammonium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.3 Example 3 (Comparative)

[0296] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g Triethylammonium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.4. Example 4 (Comparative)

[0297] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g 2,2,6,6-Tetramethylpiperidinium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.5 Example 5 (Comparative)

[0298] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g Dimethyluronium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.6 Example 6 (Comparative)

[0299] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 4 g 1,1,3,3-Tetramethylguanidinium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.7 Example 7 (Comparative)

[0300] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Triethylammonium sorbate (90% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.8 Example 8 (Comparative)

[0301] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1 g Triethylammonium sorbate (90% by weight in MEG), 2 g Triethylammonium ethylhexanoate (90% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was waxy and could not be dried through solvent extraction with scCO.sub.2.

3.9 Example 9

[0302] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 6 g MDEA, 2 g Potassium sorbate (5% by weight in MEG), 0.25 g Ammonium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.10 Example 10

[0303] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (5% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.11 Example 11

[0304] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (5% by weight in MEG), 0.5 g 2,2,6,6-Tetramethylpiperidinium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.12 Example 12

[0305] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (5% by weight in MEG), 0.25 g Dimethyluronium ethylhexanoate (70% by weight in MEG) and 6 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.13 Example 13

[0306] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (5% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (90% by weight in MEG) 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.14 Example 14

[0307] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (10% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (90% by weight MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.15 Example 15

[0308] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1 g Potassium sorbate (15% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (90% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.16 Example 16

[0309] In a polypropylene container, 48 g M200 and 1 g Graphite were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1 g Potassium sorbate (15% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (90% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.17 Example 17

[0310] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Potassium sorbate (10% by weight in MEG), 0.5 g Triethylammonium ethylhexanoate (90% by weight in MEG), 0.25 g water, 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.18 Example 18

[0311] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Triethylammonium sorbate (90% by weight in MEG), 0.5 g Dabco K 15, 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.19 Example 19

[0312] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1 g Triethylammonium sorbate (90% by weight in MEG), 1 g Dabco K 15, 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.20 Example 20

[0313] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1.5 g Potassium sorbate (10% by weight in MEG), 1 g Ammonium acetate (30% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.21 Example 21

[0314] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1.5 g Triethylammonium sorbate (90% by weight in MEG), 1 g Potassium acetate (20% by weight in MEG), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.22 Example 22

[0315] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 1.5 g Triethylammonium ethylhexanoate (90% by weight), 1 g Potassium acetate (20% by weight), 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

3.23 Example 23

[0316] In a polypropylene container, 48 g M200 were stirred in 220 g MEK at 20 C. leading to a clear solution. Similarly, 8 g MDEA, 2 g Ammonium acetate (30% by weight in MEG), 0.5 g Dabco K15, 1.5 g Exolit OP 560 and 4 g butanol were dissolved in 220 g MEK to obtain a second solution. The solutions were combined in a rectangular container (2020 cm5 cm height) by pouring one solution into the other, which led to a clear, homogeneous mixture of low viscosity. The container was closed with a lid and the mixture was gelled at room temperature for 24 h. The resulting monolithic gel slab was dried through solvent extraction with scCO.sub.2 in a 25 l autoclave leading to a porous material.

4. Results

[0317]

TABLE-US-00001 TABLE 1 Results. Thermal conductivity Compression Density [mW/m * K] strength [kg/m.sup.3] (p = 1 bar, T = 10 C.) [kPa] Example 1 (comparative) n.d. n.d. n.d. Example 2 (comparative) n.d. n.d. n.d. Example 3 (comparative) n.d. n.d. n.d. Example 4 (comparative) n.d. n.d. n.d. Example 5 (comparative) n.d. n.d. n.d. Example 6 (comparative) n.d. n.d. n.d. Example 7 (comparative) n.d. n.d. n.d. Example 8 (comparative) n.d. n.d. n.d. Example 9 127 18.1 615 Example 10 119 18.0 584 Example 11 128 17.8 422 Example 12 126 17.9 411 Example 13 121 17.3 506 Example 14 n.d. 17.4 n.d. Example 15 123 17.6 529 Example 16 n.d. 17.3 n.d. Example 17 n.d. 17.6 n.d. Example 18 124 17.4 548 Example 19 127 17.8 531 Example 20 n.d. 17.9 n.d. Example 21 n.d. 18.2 n.d. Example 22 n.d. 17.7 n.d. Example 23 n.d. 17.8 n.d.

5. Abbreviations

[0318] H.sub.2O Water [0319] K15 Dabco K15 (PUR catalyst) [0320] M200 Lupranate M200 (polyisocyanate) [0321] MEK Methyl ethyl ketone [0322] MDEA 4,4-Methylene-bis(2,6-diethylaniline)