IP Library Granted Patent US 9,296,902
Granted Patent B2
US 9,296,902 · App. 11/993,785 · Granted Mar 29, 2016

Process for modifying inorganic oxygen-containing particulate material, product obtained therefrom, and use thereof

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Quick Facts
Patent No.
US 9,296,902
App. No.
11/993,785
Granted
Mar 29, 2016
Kind
B2
Abstract

The present invention pertains to a process for preparing a modified inorganic oxygen-containing particulate material comprising the steps of: a) preparing a mixture of an aqueous suspension of inorganic oxygen-containing particulate material and an alkoxylated alcohol according to the formula (I) wherein R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5; b) optionally adding a first resin and/or a first resin precursor; c) adding one or more coupling agents to the mixture; d) optionally adding a second resin and/or a second resin precursor to the resulting mixture; and wherein optionally water is removed at least partially from the mixture before or during step b), c) or d), or after step d); and optionally converting the first resin precursor into the first resin before, during or after step c) and/or the second resin precursor into the second resin after step d).

Claims (47)

1. A process for preparing a modified colloidal silica particulate material comprising the steps of:

a) providing a de-ionised aqueous suspension of silica particulate material;

b) preparing a mixture of said de-ionised aqueous suspension of silica particulate material and an alkoxylated alcohol according to the formula

wherein R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5; and

c) adding to the mixture one or more coupling agents comprising one or more elements selected from the group consisting of Si, Al, Ti, Zr, B, Zn, Sn, and V; and allowing at least part of said one or more coupling agents to react with said silica particulate material;

wherein water is removed at least partially from the mixture during or after step c);

to obtain a suspension of modified silica particulate material in alkoxylated alcohol, said modified silica particulate material being present in an amount from 10 to 70 wt % based on the obtained suspension,

the process further comprising adding a first resin and/or a first resin precursor to the mixture from step b) prior to step c).

2. A process for preparing a modified colloidal inorganic oxygen-containing particulate material comprising the steps of:

a) preparing a mixture of an aqueous suspension of inorganic oxygen-containing particulate material and an alkoxylated alcohol according to the formula

 wherein R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5; and

b) adding to the mixture one or more coupling agents comprising one or more elements selected from the group consisting of Si, Al, Ti, Zr, B, Zn, Sn, and V; and allowing at least part of said one or more coupling agents to react with said inorganic oxygen-containing particulate material;

wherein water is removed at least partially from the mixture during or after step b); and wherein the suspension of inorganic oxygen-containing particulate material is aqueous silica which is de-ionised prior to step a);

to obtain a suspension of modified inorganic oxygen-containing particulate material in alkoxylated alcohol, said modified inorganic oxygen-containing particulate material being present in an amount from 10 to 70 wt % based on the obtained suspension,

the process further comprising adding a first resin and/or a first resin precursor to the mixture from step a) prior to step b).

3. The process according to claim 1 wherein the first resin precursor is added to the mixture in step b) and wherein the first resin precursor is converted into a resin after step b).

4. The process according to claim 1 , wherein the amount of water present in the obtained mixture is less than 5 wt %, based on the total mixture.

5. The process according to claim 2 , wherein the amount of water present in the obtained mixture is less than 2 wt %, based on the total mixture.

6. The process according to claim 2 , wherein the amount of water present in the obtained mixture is less than 1 wt %, based on the total mixture.

7. The process according to claim 2 , further comprising adding a second resin and/or a second resin precursor to the mixture after the step of obtaining a modified inorganic oxygen-containing particulate material in alkoxylated alcohol.

8. A process for preparing a modified silica particulate material comprising the steps of:

a) providing a de-ionised aqueous suspension of silica particulate material;

b) preparing a mixture of said de-ionised aqueous suspension of silica particulate material having a number average particle diameter of between 1 and 1,000 nm, an alkoxylated alcohol according to the formula

 where R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5, and one or more coupling agents comprising a silicon-based compound; and

c) allowing at least part of said one or more coupling agents to react with said silica particulate material, wherein water is removed at least partially from the mixture during or after step c);

to obtain a suspension comprising said modified silica particulate material in said alkoxylated alcohol, the process further comprising adding a first resin and/or a first resin precursor to the mixture from step b) prior to step c), said modified silica particulate material being present in an amount from 10 to 70 wt % based on the total weight of the obtained suspension.

9. The process according to claim 8 wherein the alkoxylated alcohol is selected from the group consisting of propylene glycol mono methyl ether, propylene glycol mono ethyl ether, and mixtures thereof.

10. The process according to claim 8 wherein the silicon-based compound is selected from the group consisting of silanes, disilanes, oligomers of silane, silazane, silane-functional silicones, silane-modified resins, and silsesquioxanes.

11. The process according to claim 8 wherein the number average particle diameter is between 1 and 150 nm.

12. The process according to claim 8 wherein the product resulting from the process contains less than 5 wt % of water, based on the total weight of the product.

13. A process for preparing a modified silica particulate material comprising the steps of:

a) providing a de-ionised aqueous suspension of silica particulate material;

b) preparing a mixture of said de-ionised aqueous suspension of silica particulate material, an alkoxylated alcohol according to the formula

where R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5, and one or more coupling agents;

c) allowing at least part of said one or more coupling agents to react with said silica particulate material, wherein water is removed at least partially from the mixture during or after step c);

to obtain a suspension comprising said modified silica particulate material in said alkoxylated alcohol, said modified silica particulate material being present in an amount from 10 to 70 wt % based on the total weight of the obtained suspension,

the process further comprising adding a first resin and/or a first resin precursor to the mixture from step b) prior to step c).

14. The process according to claim 13 wherein the alkoxylated alcohol is selected from the group consisting of propylene glycol mono methyl ether, propylene glycol mono ethyl ether, and mixtures thereof.

15. The process according to claim 13 wherein the coupling agent is a silicon-based compound.

16. The process according to claim 15 wherein the silicon-based compound is selected from the group consisting of silanes, disilanes, oligomers of silane, silazane, silane-functional silicones, silane-modified resins, and silsesquioxanes.

17. A process for preparing a modified inorganic oxygen-containing particulate material comprising the steps of:

a) preparing a mixture of an aqueous suspension of inorganic oxygen-containing particulate material, an alkoxylated alcohol according to the formula

where R 1 is a C 1 -C 8 alkyl, C 4 -C 8 cycloalkyl or phenyl, R 2 is hydrogen or methyl, and n is an integer from 1 to 5, and one or more coupling agents;

b) allowing at least part of said one or more coupling agents to react with said inorganic oxygen-containing particulate material, wherein water is removed at least partially from the mixture during or after step b); and

wherein the aqueous suspension of inorganic oxygen-containing particulate material is aqueous silica which is de-ionised prior to step a);

to obtain a suspension comprising said modified inorganic oxygen-containing particulate material in said alkoxylated alcohol, said modified inorganic oxygen-containing particulate material being present in an amount from 10 to 70 wt % based on the total weight of the obtained suspension, and wherein the aqueous silica which is de-ionised contains free ions in an amount of less than 1,000 ppm

the process further comprising adding a first resin and/or a first resin precursor to the mixture from step a) prior to step b).

Assignments (3)
SECURITY INTEREST Recorded Oct 1, 2018
From: STARFRUIT US MERGER SUB 1 LLC; STARFRUIT US MERGER SUB 2 LLC; AKZO NOBEL SURFACE CHEMISTRY LLC; AKZO NOBEL CHEMICALS B.V.; AKZO NOBEL CHEMICALS INTERNATIONAL B.V.
To: WILMINGTON TRUST (LONDON) LIMITED, AS COLLATERAL AGENT
Reel/Frame 047231/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 13, 2017
From: AKZO NOBEL N.V.
To: AKZO NOBEL CHEMICALS INTERNATIONAL B.V.
Reel/Frame 044427/0759 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 21, 2007
From: SCHOMAKER, ELWIN; VENDERBOSCH, RUDOLF ANTHONIUS MARIA
To: AKZO NOBEL N. V.
Reel/Frame 020284/0885 →