IP Library Granted Patent US 9,862,940
Granted Patent B2
US 9,862,940 · App. 12/523,102 · Granted Jan 9, 2018

Silica sol material for producing bilogically degradable and/or resorbable silica gel materials, the production and use thereof

Inventor: Walther Glaubitt (Wuerzburg, DE)
Assignee: BAYER INTELLECTUAL PROPERTY GMBH
C12N11/14C04B35/6224C08G77/02C08L83/02C12N5/0068D01F9/08C12N2533/10Y10T442/3976Y10T442/696
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Quick Facts
Patent No.
US 9,862,940
App. No.
12/523,102
Granted
Jan 9, 2018
Kind
B2
Abstract

The invention concerns a novel silica sol material and its use for producing bioabsorbable and biodegradable silica gel materials having improved properties. The materials such as for example fibers, fibrous nonwoven webs, powders, monoliths and/or coatings are used, for example, in medical technology and/or human medicine, in particular for wound treatment.

Claims (37)

1. A silica fibers material produced by spinning a silica sol material obtained by

a) conducting a hydrolysis condensation reaction of one silicon compound of formula (I)

SiX 4   (I)

 where the X radicals denote ethoxy groups,

under acidic catalysis at an initial pH of 0 to ≦7, in the presence or absence of a water-soluble solvent at a temperature of 0° C. to 80° C. for 24 h to 18 days,

b) then evaporating to form a single-phase solution having a viscosity ranging from 0.5 to 2 Pa·s at a shear rate of 10 s −1 at 4° C.,

c) then cooling this solution, and

d) subjecting the cold solution to a ripening to form a homogeneous sol, and

wherein 27% to 33.2% of the ethoxy groups from the tetraethoxysilane are present in the silica fibers material.

2. The silica fibers material according to claim 1 , wherein, for the acidic catalysis, the silicon compound and nitric acid acidified H 2 O are used in a molar ratio in the range of 1:1.7 to 1:1.9, and the hydrolysis condensation reaction is conducted between 20 and 60° C.

3. The silica fibers material according to claim 1 , wherein the hydrolysis condensation reaction in step a) is conducted at 20 to 60° C.

4. The silica fibers material according to claim 1 , wherein step b) proceeds in a closed apparatus at a reaction temperature of about 30 to about 90° C.

5. The silica fibers material according to claim 1 , wherein the solution in step c) is cooled down to 2° C. to 4° C.

6. The silica fibers material according to claim 1 , wherein the ripening in step d) is effected at a temperature of 2° C. to 4° C.

7. The silica fibers material according to claim 1 , wherein the ripening in step d) is carried on to a sol viscosity of 30 to 100 Pa·s at a shear rate of 10 s −1 at 4° C. and a loss factor of 2 to 5 (at 4° C., 10 l/s, 1% deformation).

8. The silica fibers material according to claim 1 , which comprises fibres, continuous filaments, fibrous nonwoven webs and/or wovens.

9. The silica fibers material according to claim 1 , wherein the conducting of the hydrolysis condensation reaction is for 3 to 8 days.

10. The silica fibers material according to claim 1 , wherein the conducting of the hydrolysis condensation reaction is with mixing at 20 rpm to 80 rpm.

11. The silica fibers material according to claim 1 , wherein the conducting of the hydrolysis condensation reaction is for 3 to 18 days.

12. A process for producing a silica fibers material by spinning a silica sol material, which is extrudable to an extent of at least 70% of the overall reaction mixture, by

a) conducting an 24 h to 18-day hydrolysis condensation reaction of one Si compounds of the formula (I)

SiX 4   (I)

 in which the X radicals denote ethoxy groups,

under acidic catalysis at an initial pH of 0 to ≦7, in the presence or absence of a water-soluble solvent at a temperature of 0° C. to 80° C.,

b) evaporating to form a single-phase solution having a viscosity ranging from 0.5 to 2 Pa·s at shear rate of 10 s −1 at 4° C.,

c) cooling single-phase solution and

d) ripening the cold solution to form a homogenous silica sol material, and

wherein 27% to 33.2% of the ethoxy groups from the tetraethoxysilane are present in the silica fibers material.

13. A method of producing a silica fibers material by spinning a silica sol material comprising:

a) conducting a hydrolysis condensation reaction of one silicon compounds of formula (I)

SiX 4   (I)

 where the X radicals denote ethoxy groups,

under acidic catalysis at an initial pH of 0 to ≦7, in the presence or absence of a water-soluble solvent at a temperature of 0° C. to 80° C. for 24 h to 18 days,

b) evaporating to form a single-phase solution having a viscosity ranging from 0.5 to 2 Pa·s at a shear rate of 10 s −1 at 4° C.,

c) cooling this solution, and

d) subjecting the cold solution to a ripening to form a homogeneous sol,

and wherein 27% to 33.2% of the ethoxy groups from the tetraethoxysilane are present in the silica fibers material.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 27, 2017
From: BAYER INNOVATION GMBH
To: BAYER INTELLECTUAL PROPERTY GMBH
Reel/Frame 044223/0686 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 24, 2010
From: GLAUBITT, WALTER
To: BAYER INNOVATION GMBH
Reel/Frame 023982/0944 →
Priority Claims (2)
DE 10 2007 002 896 · Jan 15, 2007 · national
DE 10 2007 061 873 · Dec 19, 2007 · national
Continuity (1)
Related Publication 20110183419A1 · Jul 28, 2011