# US 8,569,263 B2 · Method of producing silane-modified cationized cellulose

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- Number: US 8,569,263 B2
- Document ID: US8569263B2
- Status: Granted
- Kind: B2
- Application number: 12/673,914
- Filed: 2008-08-22
- Published: 2011-09-08
- Granted: 2013-10-29
- Earliest claimed: 2007-08-22
- Assignees: Lion Corporation
- Applicants: Youichirou Kohno; Yoko Osako; Atsushi Ito
- Inventors: Youichirou Kohno; Yoko Osako; Atsushi Ito
- Web page: https://patentgrep.com/patent/US8569263B2

## CPC

- C08B 15/06: containing nitrogen {, e.g. carbamates}
- C08B 15/05: Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur (esters or phosphorous acids C08B5/00)
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)

## Abstract

A method of producing silane-modified cationized cellulose that has excellent aqueous dispersibility, including: a step (1) of cationizing water-soluble cellulose ether in a presence of alkali in a mixed solvent of a water-compatible organic solvent to obtain slurry comprising cationized cellulose; a step (2) of adding acid to said slurry and neutralizing said alkali; a step (3) of reacting said cationized cellulose obtained after said neutralization with an aminosilane compound and a step (4) of drying the obtained slurry, wherein: drying is conducted in step (4) at 115-160° C. until weight loss on drying is 5% by weight or less, or there is also including a step (5) of adding a water-compatible organic solvent or a mixed solvent of a water-compatible organic solvent and water to the cationized cellulose after the neutralization so that water content in a whole solvent that contacts the cationized cellulose is 10% by mass or less.

## Claims

### Claim 1

A method of producing silane-modified cationized cellulose, comprising the steps of:
(1) cationizing water-soluble cellulose ether in the presence of alkali in a mixed solvent of a water-compatible organic solvent and water to obtain a slurry comprising cationized cellulose;
(2) adding acid to said slurry and neutralizing said alkali;
(3) reacting said cationized cellulose obtained after said neutralization with an aminosilane compound which is 0.3-10% by mass relative to an amount of water-soluble cellulose ether used as raw material of said cationized cellulose; and
(4) drying and powderizing the product obtained in step (3), wherein
drying is conducted in step (4) at a temperature of 115-160° C. until weight loss on drying is 5% by weight or less, or
the method further comprises the step (5) of adding a water-compatible organic solvent or a mixed solvent of a water-compatible organic solvent and water to said cationized cellulose obtained in step (2) so that the water content in the total solvent is 10% by mass or less before performing step (3).

### Claim 2 (depends on 1)

The production method according to claim 1, wherein the step (3) is conducted with an addition of an aminosilane compound to said slurry obtained in the step (2).

### Claim 3 (depends on 1)

The production method according to claim 1, wherein the step (3) is conducted with addition of an aminosilane compound to a cake obtained by conducting deliquoring treatment with respect to said slurry obtained in the step (2).

### Claim 4 (depends on 1)

The production method according to claim 1, wherein the step (5) is conducted by adding a water-compatible organic solvent or a mixed solvent of water-compatible organic solvent and water to said slurry obtained in the step (2), and mixing and agitating said slurry.

### Claim 5 (depends on 1)

The production method according to claim 1, wherein the step (5) is conducted by performing deliquoring treatment with respect to said slurry obtained in the step (2), and by adding a water-compatible organic solvent or a mixed solvent of water-compatible organic solvent and water to the obtained cake.

### Claim 6 (depends on 1)

Silane-modified cationized cellulose produced by the method of producing silane-modified cationized cellulose according to claim 1.

### Claim 7

A method of producing silane-modified cationized cellulose, comprising the steps of:
(1) cationizing water-soluble cellulose ether in the presence of alkali in a mixed solvent of a water-compatible organic solvent and water to obtain a slurry comprising cationized cellulose:
(2) adding acid to said slurry and neutralizing said alkali;
(3) reacting said cationized cellulose obtained after said neutralization with an aminosilane compound which is 0.9-10% by mass relative to an amount of water-soluble cellulose ether used as raw material of the cationized cellulose; and
(4) drying and powderizing the product obtained in step (3) at a temperature of 115-160° C. until weight loss on drying is 5% by weight or less.

### Claim 8

A method of producing silane-modified cationized cellulose, comprising the steps of:
(1) cationizing water-soluble cellulose ether in the presence of alkali in a mixed solvent of a water-compatible organic solvent and water to obtain a slurry comprising cationized cellulose;
(2) adding acid to said slurry and neutralizing said alkali;
(3) reacting said cationized cellulose obtained after said neutralization with an aminosilane compound which is 0.3-10% by mass relative to an amount of water-soluble cellulose ether used as raw material of the cationized cellulose;
(4) drying and powderizing the product obtained in step (3), and
(5) adding a water-compatible organic solvent or a mixed solvent of a water-compatible organic solvent and water to said cationized cellulose obtained in step (2) so that the water content in the total solvent is 10% by mass or less before performing step (3).

### Claim 9 (depends on 7)

The method according to claim 7, wherein step (3) is conducted with an addition of an aminosilane compound to said slurry obtained in step (2).

### Claim 10 (depends on 7)

The method according to claim 7, wherein step (3) is conducted with addition of an aminosilane compound to a cake obtained by conducting deliquoring treatment with respect to said slurry obtained in step (2).

### Claim 11 (depends on 8)

The method according to claim 8, wherein step (3) is conducted with an addition of an aminosilane compound to said slurry obtained in step (2).

### Claim 12 (depends on 8)

The method according to claim 8, wherein step (3) is conducted with addition of an aminosilane compound to a cake obtained by conducting deliquoring treatment with respect to said slurry obtained in step (2).

### Claim 13 (depends on 8)

The method according to claim 8, wherein step (5) is conducted by adding a water-compatible organic solvent or a mixed solvent of water-compatible organic solvent and water to said slurry obtained in step (2), and mixing and agitating said slurry.

### Claim 14 (depends on 8)

The method according to claim 8, wherein step (5) is conducted by performing deliquoring treatment with respect to said slurry obtained in step (2), and by adding a water-compatible organic solvent or a mixed solvent of water-compatible organic solvent and water to the obtained cake.
