Process for producing porous materials

Patent metadata

Field	Value
Publication number	US-10240020-B2
Application number	US-201414893602-A
Country	US
Kind code	B2
Filing date	May 14, 2014
Priority date	May 24, 2013
Publication date	Mar 26, 2019
Grant date	Mar 26, 2019

Abstract

The present invention relates to a process for producing porous materials, which comprises providing a mixture comprising a composition (A) comprising components suitable to form an organic gel and a solvent mixture (B), reacting the components in the composition (A) in the presence of the solvent mixture (B) to form a gel and drying of the gel, wherein the solvent mixture (B) is a mixture of at least two solvents and the solvent mixture has a Hansen solubility parameter δH in the range of 3.0 to 5.0 MPa-1, determined using the parameter δH of each solvent of the solvent mixture (B). 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.

First claim

The invention claimed is:

1. A process for preparing a porous material, comprising:
a) providing a mixture (I) comprising
(i) a composition (A) comprising components suitable to form an organic gel and
(ii) a solvent mixture (B),

b) reacting the components in the composition (A) in the presence of the solvent mixture (B) to form a gel, and
c) drying of the gel obtained in step b),
wherein:
the solvent mixture (B) is a mixture of at least two solvents;
the solvent mixture (B) comprises propylene carbonate as one of the at least two solvents; and
the solvent mixture (B) has a Hansen solubility parameter δ H in the range of 3.0 to 5.0 MPa −1 , determined using the parameter δ H of each solvent of the solvent mixture (B).

2. The process according to claim 1 , wherein the composition (A) comprises at least one polyfunctional isocyanate as component (a1).

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

4. The process according to claim 3 , wherein the at least one aromatic amine is a polyfunctional aromatic amine.

5. The process according to claim 3 , wherein the at least one aromatic amine (a2) has the general formula I

where R 1 and R 2 can be identical or different and are each selected independently from among hydrogen and linear or branched alkyl groups having from 1 to 6 carbon atoms and all substituents Q 1 to Q 5 and Q 1′ to Q 5′ are identical or different and are each selected independently from among hydrogen, a primary amino group and a linear or branched alkyl group having from 1 to 12 carbon atoms, where the alkyl group can bear further functional groups, with the proviso that the compound having the general formula I comprises at least two primary amino groups, where at least one of Q 1 , Q 3 and Q 5 is a primary amino group and at least one of Q 1′ , Q 3′ and Q 5′ is a primary amino group.

6. The process according to claim 1 , wherein composition (A) comprises:
(a1) from 25 to 94.9% by weight of at least one polyfunctional isocyanate, and
(a2) from 0.1 to 30% by weight of at least one polyfunctional aromatic amine having the general formula I

where R 1 and R 2 can be identical or different and are each selected independently from among hydrogen and linear or branched alkyl groups having from 1 to 6 carbon atoms and all substituents Q 1 to Q 5 and Q 1′ to Q 5′ are identical or different and are each selected independently from among hydrogen, a primary amino group and a linear or branched alkyl group having from 1 to 12 carbon atoms, where the alkyl group can bear further functional groups, with the proviso that the compound having the general formula I comprises at least two primary amino groups, where at least one of Q 1 , Q 3 and Q 5 is a primary amino group and at least one of Q 1′ , Q 3′ and Q 5′ is a primary amino group,
(a3) from 0 to 15% by weight of water, and
(a4) from 0.1 to 30% by weight of at least one catalyst,
in each case based on the total weight of the components (a1) to (a4), where the % by weight of the components (a1) to (a4) add up to 100% by weight.

7. The process according to claim 3 , wherein the amine component (a2) comprises at least one 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.

8. The process according to claim 3 , wherein component (a4) is selected from the group consisting of primary, secondary and tertiary amines, triazine derivatives, metal-organic compounds, metal chelates, oxides of phospholenes, quaternary ammonium salts, ammonium hydroxides and alkali metal and alkaline earth metal hydroxides, alkoxides and carboxylates.

9. The process according to claim 3 , wherein component (a4) is selected from the group consisting of dimethylcyclohexylamine, bis(2-dimethylaminoethyl) ether, N,N,N,N,N-pentamethyldiethylenetriamine, methylimidazole, dimethylimidazole, aminopropylimidazole, dimethylbenzylamine, 1,6-diazabicyclo[5.4.0]undec-7-ene, trisdimethylaminopropylhexahydrotriazine, triethylamine, tris(dimethylaminomethyl)phenol, triethylenediamine (diazabicyclo[2.2.2]octane), dimethylaminoethanolamine, dimethylaminopropylamine, N,N-dimethylaminoethoxyethanol, N,N,N-trimethylaminoethylethanolamine, triethanolamine, diethanolamine, triisopropanolamine, diisopropanolamine, methyldiethanolamine, butyldiethanolamine, metal acetylacetonates, ammonium ethylhexanoates and metal ethylhexanoates.

10. The process according to claim 3 , wherein the catalyst catalyzes the trimerization to form isocyanurate groups.

11. The process according to claim 3 , wherein component (a4) comprises at least one tertiary amino group.

12. The process according to claim 1 , wherein no water is used.

13. The process according to claim 1 , wherein at least 0.1% by weight of water is added.

14. The process according to claim 1 , wherein the solvent mixture (B) has a Hansen solubility parameter δ P in the range of 7.5 to 10.0 MPa −1 , determined using the parameter δ P of each solvent of the solvent mixture (B).

15. The process according to claim 1 , wherein the solvent mixture (B) has a Hansen solubility parameter δ D in the range of 15.0 to 18.0 MPa −1 , determined using the parameter δ D of each solvent of the solvent mixture (B).

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

17. The process according to claim 1 , wherein the drying according to step c) is carried out under supercritical conditions.

Assignees

• Basf Se

Inventors

• Fricke Marc
• Weinrich Dirk

Classifications

• C08J2205/028

  Xerogel, i.e. an air dried gel · CPC title

• C08J2375/02

  Polyureas · CPC title

• C08J2201/0502

  the liquid phase being organic · CPC title

• C08G2101/0091

  Chemistry & Metallurgy · mapped topic

• C08J2205/026

  Aerogel, i.e. a supercritically dried gel · CPC title