# US 10,865,280 B2 · Method of producing films from high consistency enzyme fibrillated nanocellulose

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- Number: US 10,865,280 B2
- Document ID: US10865280B2
- Status: Granted
- Kind: B2
- Application number: 16/066,687
- Filed: 2016-12-30
- Published: 2019-01-03
- Granted: 2020-12-15
- Earliest claimed: 2015-12-31
- Assignees: Teknologian tutkimuskeskus VTT Oy
- Applicants: Teknologian tutkimuskeskus VTT Oy
- Inventors: Vesa Kunnari; Jaakko Pere; Jaakko Hiltunen; Katariina Kemppainen
- Web page: https://patentgrep.com/patent/US10865280B2

## CPC

- C08J 5/18: Manufacture of films or sheets
- C08L 1/02: Cellulose; Modified cellulose
- D21C 5/005: {Treatment of cellulose-containing material with microorganisms or enzymes}
- D21H 11/18: Highly hydrated, swollen or fibrillatable fibres
- D21H 11/20: Chemically or biochemically modified fibres
- D21H 17/26: Ethers thereof
- D21H 17/31: Gums
- D21H 17/36: Polyalkenyalcohols; Polyalkenylethers; Polyalkenylesters
- C08J 2301/02: Cellulose; Modified cellulose
- C08L 2203/16: used for films
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- D21C: PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21H: PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR

## Abstract

According to an example aspect of the present invention, there is provided a method of producing films from nanocellulose based raw materials having high consistency and thereby providing low energy consuming and feasible manufacturing process of CNF films and film materials.

## Claims

### Claim 1

A method for producing a film from enzyme fibrillated nanocellulose raw material, the method comprising:
mixing the enzyme fibrillated nanocellulose raw material with additives and forming a fiber web, wherein the enzyme fibrillated nanocellulose raw material comprises a consistency of between 15% and 40%,
laying the fiber web onto a metal substrate, wherein the laying of the fiber web is carried out by extrusion,
drying the fiber web on the metal substrate and forming a film material, wherein the film material adheres to the metal substrate to prevent shrinkage of the film material,
delaminating the film material from the metal substrate,
rewinding the film material onto a roll, and
calandering the film material from the roll and forming a film having a desired thickness;
wherein the additives comprise TEMPO-oxidized cellulose nanofibrils, and wherein the TEMPO-oxidized cellulose nanofibrils are present in an amount of 1-2% by dry weight of the fiber web.

### Claim 2 (depends on 1)

The method of claim 1, wherein the enzyme fibrillated nanocellulose raw material has a consistency of between 20% and 30%.

### Claim 3 (depends on 1)

The method of claim 1, wherein the thickness of the film is adjusted to between 20 μm and 500 μm.

### Claim 4 (depends on 1)

The method of claim 1, wherein the additives further comprise an additional bio-based polymer.

### Claim 5 (depends on 1)

The method of claim 1, wherein the method is continuous.

### Claim 6 (depends on 1)

The method of claim 1, wherein the thickness of the film is adjusted to between 20 μm and 200 μm.

### Claim 7 (depends on 1)

The method of claim 1, wherein the drying is done for 10 hours or less.

### Claim 8 (depends on 1)

The method of claim 1, wherein the enzyme fibrillated nanocellulose raw material has a consistency of between 20% and 30%, and wherein the drying is done for a period of 4 to 5 hours.

### Claim 9 (depends on 1)

The method of claim 1, wherein the additives further comprise a member selected from the group consisting of glycerol, carboxymethylated cellulose, carrageenan, and polyvinyl alcohol.

### Claim 10

A method for producing a film from enzyme fibrillated nanocellulose raw material comprising:
mixing an enzyme fibrillated nanocellulose raw material having a consistency of between 15% and 40% with a bio-based polymer to form a fiber web,
extruding the fiber web onto a metal substrate,
drying the fiber web on the metal substrate to form a film material, wherein the film material adheres to the metal substrate to prevent shrinkage of the film material, and
delaminating the film material from the metal substrate to provide the film;
wherein the bio-based polymer comprises TEMPO-oxidized cellulose nanofibrils, and wherein the TEMPO-oxidized cellulose nanofibrils are present in an amount of 1-2% by dry weight of the fiber web.

### Claim 11 (depends on 10)

The method of claim 10, wherein the enzyme fibrillated nanocellulose raw material has a consistency of between 20% and 30%.

### Claim 12 (depends on 10)

The method of claim 10, wherein the extruding is carried out at a temperature of 25° C.