Method for producing nanofibrillar cellulose and nanofibrillar cellulose product

Patent metadata

Field	Value
Publication number	US-11274396-B2
Application number	US-202015930962-A
Country	US
Kind code	B2
Filing date	May 13, 2020
Priority date	Mar 31, 2014
Publication date	Mar 15, 2022
Grant date	Mar 15, 2022

Abstract

In a method for producing nanofibrillar cellulose, cellulose based fibre material, in which internal bonds in cellulose fibres have been weakened by 5 preliminary modification of cellulose, is subjected to disintegration treatment in form of pulp comprising fibres and liquid. The fibre material is supplied at a consistency higher than 10 wt-%, preferably at least 15 wt-%, to a disintegration treatment where fibrils are detached from the fibre material by joint effect of repeated impacts to the fibre material by fast moving 10 successive elements and the weakened internal bonds of the cellulose fibres. The nanofibrillar cellulose is withdrawn from the disintegration treatment at dry matter which is equal or higher than the consistency of the fibre material.

First claim

The invention claimed is:

1. A nanofibrillar cellulose product, which is in the form of moist powder containing particles formed of cellulose nanofibrils wherein a dry matter content of the moist nanofibrillar cellulose powder is between 16-60 wt-% based on the dry matter of nanofibrils, where a cellulose in a fibrous starting material is chemically modified cellulose and the median particle diameter of the nanocellulose powder by laser diffraction analysis is 100-1000 micrometers, wherein the cellulose is
oxidized cellulose having carboxylate content of at least 0.8 mmol/g or higher,
carboxymethylated cellulose having degree of substitution above 0.1, or
cationized cellulose having degree of substitution of at least 0.1 or higher;
wherein the nanofibrillar cellulose product is obtained directly after a disintegration treatment of cellulose.

2. The nanofibrillar cellulose product according to claim 1 , wherein when dispersed to a concentration of 0.1 wt-% in water, the turbidity of the nanofibrillar cellulose aqueous dispersion is lower than 80 NTU, measured by nephelometry.

3. The nanofibrillar cellulose product according to claim 1 , wherein when dispersed to a concentration of 0.1 wt-% in water, the turbidity of the nanofibrillar cellulose aqueous dispersion is from 10 to 60 NTU, measured by nephelometry.

4. The nanofibrillar cellulose product according to claim 1 , wherein the dry matter content of the nanofibrillar cellulose powder is between 20-35 wt-% based on the dry matter of nanofibrils.

5. The nanofibrillar cellulose product according to claim 1 , wherein the dry matter content of the nanofibrillar cellulose powder is between 22-30 wt-% based on the dry matter of nanofibrils.

6. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is ionically charged cellulose.

7. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is
oxidized cellulose having carboxylate content of at least 0.95 mmol/g or higher,
carboxymethylated cellulose having degree of substitution of at least 0.12 or higher, or
cationized cellulose having degree of substitution of at least 0.15 or higher.

8. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is
oxidized cellulose having carboxylate content of at least 1.00 mmol/g or higher,
carboxymethylated cellulose having degree of substitution in the range of 0.12-0.2, or
cationized cellulose having degree of substitution in the range of 0.1-0.6.

9. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is
oxidized cellulose having carboxylate content in the range 0.8-1.8 mmol/g, or
cationized cellulose having degree of substitution between 0.15-0.35.

10. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is
oxidized cellulose having carboxylate content between 0.95-1.65 mmol/g.

11. The nanofibrillar cellulose product according to claim 10 , wherein when dispersed to a concentration of 0.5% in water, it has a yield stress is between 3 to 20 Pa.

12. The nanofibrillar cellulose product according to claim 1 , wherein the cellulose is
oxidized cellulose having carboxylate content between 1.00-1.55 mmol/g.

13. The nanofibrillar cellulose product according to claim 1 , wherein when dispersed to a concentration of 0.5% in water, it has a zero shear viscosity of 1,000 to 50,000 Pa·s and a yield stress of 1 to 50 Pa.

14. The nanofibrillar cellulose product according to claim 1 , comprising fibrils or fibril bundles having a number-average diameter below 200 nm and a length exceeding one micrometer.

15. A medical product comprising the nanofibrillar cellulose product according to claim 1 .

16. A cosmetic product comprising the nanofibrillar cellulose product according to claim 1 .

17. The nanofibrillar cellulose product according to claim 1 , wherein when dispersed to a concentration of 0.5% in water, it has a zero shear viscosity of 5,000 to 50,000 Pa·s and a yield stress of 3 to 30 Pa.

18. The nanofibrillar cellulose product according to claim 1 , wherein in the moist powder the fibrils of the nanofibrillar cellulose are gathered to moist cellulose particles aggregated due to moisture dependent stickiness of the particles.

19. The nanofibrillar cellulose product according to claim 1 , wherein the nanofibrillar cellulose is obtained by a method comprising:
preparing cellulose based fibre material, in which internal bonds in cellulose fibres have been weakened by preliminary chemical modification of cellulose, in form of pulp suspension comprising fibres and liquid, wherein cellulose based fibre material, in which internal bonds in cellulose fibres have been weakened by preliminary chemical modification of cellulose, is subjected to disintegration treatment in form of pulp suspension comprising fibres and liquid
supplying the pulp suspension at a consistency higher than 10 wt-% based on the proportion of the fibres in the pulp suspension, to a disintegration treatment;
detaching fibrils from the fibre material in course of said disintegration treatment by joint effect of repeated impacts to the fibre material by fast moving successive elements and the weakened internal bonds of the cellulose fibres; and
withdrawing the nanofibrillar cellulose from the disintegration treatment at dry matter which is equal or higher than the consistency of the fibre material.

20. The nanofibrillar cellulose product according to claim 17 , wherein the fibre material supplied to the disintegration treatment is ionically charged cellulose having one of the following properties:
oxidized cellulose having carboxylate content of at least 0.8 mmol/g pulp or higher,
carboxymethylated cellulose having degree of substitution above 0.1, or
cationized cellulose having degree of substitution of at least 0.1 or higher.

21. The nanofibrillar cellulose product according to claim 17 , wherein the pulp suspension is subjected to the disintegration treatment having a content of gas of greater than 10 volume percent.

22. The nanofibrillar cellulose product according to claim 17 , wherein the disintegrating treatment, the fibre material is subjected to repeated impacts successively from opposite directions.

Assignees

• Upm—Kymmene Corp
• Upm Kymmene Corp

Inventors

• Nuopponen Markus
• Tamper Juha
• Kajanto Isko

Classifications

• D21D1/36 Primary

  with vertical shaft · CPC title

• D21H11/18

  Highly hydrated, swollen or fibrillatable fibres · CPC title

• D21H11/20 Primary

  Chemically or biochemically modified fibres · CPC title

• D21B1/14 Primary

  Disintegrating in mills · CPC title