POROUS MATERIALS WITH SUPERIOR REVERSIBLE WATER UPTAKE

Abstract

A process for preparing a porous material, including the steps of providing a mixture (I) containing a composition (A) containing 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), wherein the composition (A) contains at least one compound (af) containing phosphorous and at least one functional group which is reactive towards isocyanates and at least one component (au) selected from the group consisting of urea, biuret, and derivatives of urea and biuret.

Claims

1. A process for preparing a porous material, the process comprising: reacting the components in the a composition (A) in the presence of a solvent (B) to form a gel, and drying the gel obtained in step b), wherein the composition (A) comprises a compound (af) comprising phosphorous and a functional group which is reactive towards isocyanates and a compound (au) selected from the group consisting of urea, biuret, and derivatives of urea and biuret.

2. The process according to claim 1, wherein the compound (au) is selected from the group consisting of urea, dimethyl urea, diphenyl urea, ethylene urea, dihydroxy ethylene urea, propylene urea, and biuret.

3. The process according to claim 1, wherein the composition (A) corrrprises the compound (af) in an amount which results in a phosphorous content in the porous material in a range of from 1 to 20% by weight.

4. The process according to claim 1, wherein the composition (A) comprises the compound (au) in an amount in the range of from 0.1 to 15% by weight.

5. The process according to claim 1, wherein the compound (af) comprises a functional group comprising phosphorous.

6. The process according to claim 5, wherein the compound (af) comprises a functional group comprising phosphorous selected from the group consisting of a phosphate, a phosphonate, a phosphinate, a phosphite, a phosphonite, a phosphinite, and a phosphine oxide.

7. The process according to claim 1, wherein the composition (A) further comprises a catalyst system (CS) comprising a catalyst component (Cl) selected from the group consisting of an alkali metal and an earth alkali metal, ammonium, an ionic liquid salt of a saturated or unsaturated monocarboxylic acid.

8. The process according to claim 1, wherein the composition (A) further comprises a polyfunctional isocyanate as component (a1), and an aromatic amine as component (a2), optionally comprises water as component (a3), and optionally comprises at least one catalyst as component (a4).

9. The process according to claim 1, wherein the drying is carried out by converting liquid comprised in the gel into a gaseous state at a temperature and a pressure below a critical temperature and a critical pressure of the liquid comprised in the gel.

10. The process according to claim 1, wherein the drying is carried out under supercritical conditions.

11. A porous material, obtained by the process according to claim 1.

12. An insulation material or adsorption material, comprising the porous material according to claim 11.

13. The insulation material or adsorption material according to claim 12, wherein the porous material is used in interior or exterior insulation systems.

14. A method for removing a mold in the insulation material or adsorption according to claim 12, the method comprising: removing the mold with the porous material.

Description

EXAMPLES

1. Methods

1.1 Determination of Thermal Conductivity

[0294] The thermal conductivity was measured according to DIN EN 12667 with a heat flow meter from Hesto (Lambda Control A50).

1.2 Determination of Compressive Strength and E Modulus

[0295] The compressive strength and the elastic modulus was measured according to DIN 53421 with 10% strain.

1.3 Determination of the Water Uptake

[0296] The mass of a sample was determined before and after soaking it completely under water for 24 hours. The water uptake was calculated accordingly in relation to the weight of the sample. After drying the sample for 24 hours at room temperature the shrinkage and the surface appearance was investigated.

2. Materials

[0297] 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 2100 mPa.Math.s at 25 C. in accordance with DIN 53018 (hereafter M200) [0298] Component a2: 3,3,5,5-Tetraethyl-4,4diaminodiphenylmethane (hereinafter MDEA) [0299] Catalyst: Triethanolamine Urea dissolved in monoethylene glycol (20%) [0300] Flame redardant:Exolit OP560

3. Examples

[0301] Water uptake 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)

[0302] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 2 g urea solution and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.2 Example 2 (Comparative)

[0303] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.3 Example 3 (Comparative)

[0304] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 1g OP 560 and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.4 Example 4

[0305] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 2 g urea solution, 1 g OP560 and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.5 Example 5

[0306] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 2 g urea solution, 2 g OP560 and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.6 Example 6

[0307] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 4 g urea solution, 2 g OP560 and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

3.7 Example 7

[0308] In a polypropylene container, 48 g M200 were dissolved under stirring in 210 g acetone at 20 C. leading to a clear solution. Similarly, 2 g MDEA, 4 g TEOA, 2 g urea solution, 8 g OP560 and 4 g water were dissolved in 210 g acetone 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 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 for 7 days at ambient conditions leading to a porous material.

4. Results

[0309]

TABLE-US-00001 TABLE 1 Results Compressive strength [kPa] Water Density E modulus uptake [kg/m.sup.3] [N/mm.sup.2] [wt %] Example 1 (comparative) 105 251 43 2 g MDEA, 2 g TEOA, 2 g urea 1.62 solution, 4 g water) Example 2 (comparative) 109 297 3 2 g MDEA, 2 g TEOA, 4 g water 2.92 Example 3 (comparative) 2 g MDEA, 106 295 10 2 g TEOA, 4 g water + 1 g OP560 3.02 Example 4 2 g MDEA, 2 g TEOA, 113 384 140 2 g urea solution, 4 g Wasser + 1 g 8.98 OP560 Example 5 2 g MDEA, 2 g TEOA, 115 383 322 2 g urea solution, 4 g Wasser + 2 g 9.75 OP560 Example 6 2 g MDEA, 2 g TEOA, 119 377 590 2 g urea solution, 4 g Wasser + 4 g 9.55 OP560 Example 7 2 g MDEA, 2 g TEOA, 125 379 728 2 g urea solution, 4 g Wasser + 8 g 8.19 OP560

5. Abbreviations

[0310] H.sub.2O Water

[0311] TEOA Triethanolamine (PUR catalyst)

[0312] Urea solution urea dissolved in monoethylene glycol

[0313] M200 Lupranate M200 (polyisocyanate)

[0314] MEK Methyl ethyl ketone

[0315] MDEA 4,4-Methylene-bis(2,6-diethylaniline)

LITERATURE CITED

[0316] WO 95/02009 A1

[0317] WO 2008/138978 A1

[0318] WO 2011/069959 A1

[0319] WO 2012/000917 A1

[0320] WO 2012/059388 A1

[0321] PCT/EP2017/05094

[0322] Polyurethane, 3.sup.rd edition, G. Oertel, Hanser Verlag, Munich, 1993

[0323] WO 00/24799 A1

[0324] Plastics Additive Handbook, 5th edition, H. Zweifel, ed. Hanser Publishers, Munich, 2001

[0325] WO 2009/027310 A1