IP Library Granted Patent US 10,017,621
Granted Patent B2
US 10,017,621 · App. 15/312,541 · Granted Jul 10, 2018

Process for producing porous alginate-based aerogels

Inventors: Marc Fricke (Osnabrueck, DE); Dirk Weinrich (Osnabrueck, DE); Wibke Loelsberg (Osnabrueck, DE); Raman Subrahmanyam (Hamburg, DE); Irina Smirnova (Hamburg, DE); Pavel Gurikov (Hamburg, DE)
Assignee: BASF SE
C08J9/28C08J9/0066C08J9/122C08J9/35C09K5/14C08J2201/026C08J2201/05C08J2201/0502C08J2203/06C08J2205/022C08J2205/024C08J2205/026C08J2205/028C08J2205/042C08J2305/04C08J2483/00
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Quick Facts
Patent No.
US 10,017,621
App. No.
15/312,541
Granted
Jul 10, 2018
Kind
B2
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 water soluble polysaccharide, at least one compound suitable to react as cross-linker for the polysaccharide or to release a cross-linker for the polysaccharide, and water, and preparing a gel (A) comprising exposing mixture (I) to carbon dioxide at a pressure in the range of from 20 to 100 bar for a time sufficient to form a gel (A), and depressurizing the gel (A). Gel (A) subsequently is exposed to a water miscible solvent (L) to obtain a gel (B), which is dried. 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, for cosmetic applications, for biomedical applications or for pharmaceutical applications.

Claims (24)

1. A process for preparing a porous material, the process comprising:

a) providing a mixture (I) comprising

(i) a water soluble polysaccharide,

(ii) a compound which reacts as a cross-linker for the polysaccharide or which releases a cross-linker for the polysaccharide, and

(iii) water;

b) preparing a gel (A) by a process comprising

b1) exposing the mixture (I) to carbon dioxide at a pressure in a range of from 20 to 100 bar for a time sufficient to form a gel (A), and

b2) depressurizing the gel (A);

c) exposing the gel (A) to a water miscible solvent (L) to obtain a gel (B); and

d) drying of the gel (B).

2. The process according to claim 1 , wherein the water soluble polysaccharide is selected from the group consisting of agar, alginate, carrageenan, cellulose, hyaluronic acid, pectin, starch, xanthan gum, modified cellulose, chitin, chitosan, and a mixture thereof.

3. The process according to claim 1 , wherein the water soluble polysaccharide is an alginate.

4. The process according to claim 1 , wherein the preparing in b) is carried out at a temperature in a range of from 10 to 40° C.

5. The process according to claim 1 , wherein carbon dioxide in the exposing in b1) is gaseous.

6. The process according to claim 1 , wherein the compound which reacts as a cross-linker for the polysaccharide or which releases a cross-linker for the polysaccharide is selected from the group consisting of a carbonate having no hydroxyl group, a hydroxy carbonate, and a mixture thereof.

7. The process according to claim 1 , wherein the compound which reacts as a cross-linker for the polysaccharide or which releases a cross-linker for the polysaccharide in the mixture (I) comprises calcium carbonate.

8. The process according to claim 1 , wherein the solvent (L) is selected from the group consisting of an ether, an ester, an alcohol, a ketone, an aldehyde, an alkyl alkanoate, an amide, a sulfoxide, an organic carbonate, an aliphatic and cycloaliphatic halogenated hydrocarbon, a halogenated aromatic compound, a fluorine-containing ether, and a mixture thereof.

9. The process according to claim 1 , wherein the solvent (L) is selected from the group consisting of a C1 to C6 alcohol, a C1 to C6 ketone, and a mixture thereof.

10. The process according to claim 1 , wherein a water insoluble solid (S) is added to the mixture (I).

11. The process according to claim 1 , wherein a compound (C) is added to the mixture (I) in the providing in a), wherein the compound (C) is selected from the group consisting of a natural hydrocolloid-forming polymer, a synthetic hydrocolloid-forming polymer, and a mixture thereof.

12. The process according to claim 1 , wherein the exposing in c) is carried out at a pressure in a range of from 10 to 100 bar.

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

14. The process according to claim 1 , wherein the drying in d) is carried out under supercritical conditions.

15. The process according to claim 3 , wherein the alginate has an average particle size of no more than about 0.2 mm and a viscosity, in an 1% aqueous solution at a pH 7 and at 20° C., of from 300 to 800 mPas.

Assignments (7)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 21, 2026
From: AEROGEL-IT
To: EXUUD, INC.
Reel/Frame 075338/0990 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 4, 2023
From: BASF SE
To: AEROGEL-IT GMBH
Reel/Frame 064496/0266 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2018
From: SUBRAHMANYAM, RAMAN; GURIKOV, PAVEL
To: TUTECH INNOVATION GMBH
Reel/Frame 045751/0549 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2018
From: TECHNISCHE UNIVERSITAET HAMBURG-HARBURG; TUTECH INNOVATION GMBH
To: BASF POLYURETHANES GMBH
Reel/Frame 045755/0142 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 9, 2018
From: BASF POLYURETHANES GMBH
To: BASF SE
Reel/Frame 045755/0149 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 22, 2017
From: FRICKE, MARC; WEINRICH, DIRK; LOELSBERG, WIBKE
To: BASF POLYURETHANES GMBH
Reel/Frame 044199/0578 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 22, 2017
From: SUBRAHMANYAM, RAMAN; SMIRNOVA, IRINA; GURIKOV, PAVEL
To: TECHNISCHE UNIVERSITAET HAMBURG-HARBURG
Reel/Frame 044199/0569 →
Priority Claims (1)
EP 14168810 · May 19, 2014 · regional
Continuity (1)
Related Publication 20170081494A1 · Mar 23, 2017
Cited By (2)
US 12,189,260 US 12,607,896