Process for producing porous materials

Patent metadata

Field	Value
Publication number	US-10717841-B2
Application number	US-201515128515-A
Country	US
Kind code	B2
Filing date	Mar 24, 2015
Priority date	Mar 24, 2014
Publication date	Jul 21, 2020
Grant date	Jul 21, 2020

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 at least one monool (am) and 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). 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.

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 a monool (am) and a composition (A*) comprising: a polyfunctional isocyanate as component (a1), at least one aromatic amine as component (a2), optionally, water as component (a3), and optionally at least one catalyst as component (a4); and
(ii) a solvent (B),
b) reacting the components of the composition (A) in the solvent (B) to form a mixture of an organic gel in the solvent (B), and c) drying of the mixture to remove the solvent (B) and obtain the organic gel as the porous material obtained in b),
wherein
the at least one aromatic amine (a2) is a polyfunctional aromatic amine,
the monool is present in the composition (A) in an amount of from 0.5 to 25% by weight based on the composition (A).

2. The process according to claim 1 , wherein the monool is selected from the group consisting of aliphatic monools with 1 to 20 carbon atoms and aromatic monools with 1 to 20 carbon atoms.

3. The process according to claim 1 , 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 the group consisting of 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 the group consisting of 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.

4. The process according to claim 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 the group consisting of 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 the group consisting of 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,
(a4) from 0.1 to 30% by weight of at least one catalyst, and
in each case based on the total weight of the components (a1), (a2), (a3), and (a4), where the % by weight of the components (a1), (a2), (a3), and (a4) add up to 100% by weight.

5. The process according to claim 1 , 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 the group consisting of linear or branched alkyl groups which have from 1 to 12 carbon atoms and can bear further functional groups.

6. The process according to claim 1 , wherein component (a4) is present and 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.

7. The process according to claim 1 , wherein at least one catalyst as component (a4) is present and the catalyst (a4) catalyzes trimerization of the at least one polyfunctional isocyanate to form isocyanurate groups.

8. The process according to claim 1 , wherein at least 0.1% by weight of water as component (a3) is added.

9. The process according to claim 1 , wherein the drying according to 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.

10. A porous material, which is obtained by the process according to claim 1 .

11. The porous material according to claim 10 , wherein the drying according to c) is carried out under supercritical conditions.

12. A thermal insulation material or a vacuum insulation panel comprising the porous material according to claim 10 .

13. An interior or exterior thermal insulation system comprising the thermal insulation material or the vacuum insulation panel according to claim 12 .

Assignees

• Basf Se

Inventors

• Fricke Marc
• Weinrich Dirk
• Loelsberg Wibke

Classifications

• F16L59/065

  using vacuum (F16L59/075 takes precedence) · CPC title

• C08J2201/0502

  the liquid phase being organic · CPC title

• C08J9/286 Primary

  the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers · CPC title

• C08J9/28 Primary

  by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum · CPC title

• C08J3/12

  Powdering or granulating · CPC title