# US 2019/0169377 A1 · Method for producing master batch

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- Number: US 2019/0169377 A1
- Document ID: US20190169377A1
- Status: Published application
- Kind: A1
- Application number: 16/315,220
- Filed: 2017-07-11
- Published: 2019-06-06
- Earliest claimed: 2016-07-11
- Assignees: Nippon Paper Industries Co., Ltd.
- Applicants: Nippon Paper Industries Co., Ltd.
- Inventors: Yusuke Yasukawa; Kotaro Ito; Takeshi Nakayama; Kazuhiko Ishizuka
- Web page: https://patentgrep.com/patent/US20190169377A1

## CPC

- C08J 3/22: using masterbatch techniques
- C08J 3/226: {using a polymer as a carrier}
- C08B 15/04: Carboxycellulose, e.g. prepared by oxidation with nitrogen dioxide
- C08H 8/00: Macromolecular compounds derived from lignocellulosic materials {(pretreatment thereof B27N)}
- C08J 5/18: Manufacture of films or sheets
- C08L 1/02: Cellulose; Modified cellulose
- C08L 7/00: Compositions of natural rubber
- C08L 7/02: Latex
- C08L 21/00: Compositions of unspecified rubbers
- D21C 9/007: {by mechanical or physical means}
- D21H 11/18: Highly hydrated, swollen or fibrillatable fibres
- G01N 21/94: Investigating contamination, e.g. dust (G01N21/85 takes precedence)
- C08J 2301/02: Cellulose; Modified cellulose
- C08J 2321/02: Latex
- C08J 2407/02: Latex
- C08L 2203/16: used for films
- C08L 2205/16: Fibres; Fibrils
- C08L 2312/00: Crosslinking
- 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)
- 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)
- C08H: DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS (polysaccharides C08B; natural rubber C08C; natural resins or their derivatives C09F; bituminous materials C10)
- 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
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

A process for preparing a master batch, comprising: the step of filtrating a dispersion of cellulose nanofibers under pressure or under reduced pressure with a filtration pressure differential of 0.01 MPa or more; and the step of mixing cellulose nanofibers obtained by the filtration step and rubber component is provided. A master batch can be provided to provide a rubber composition with improved mechanical strengths by the invention.

## Claims

### Claim 1

A process for preparing a master batch, comprising:
the step of filtrating a dispersion of cellulose nanofibers under pressure or under reduced pressure with a filtration pressure differential of 0.01 MPa or more; and
the step of mixing cellulose nanofibers obtained by the filtration step and rubber component.

### Claim 2 (depends on 1)

The process of claim 1, wherein a filtration aid is used in the filtration step.

### Claim 3 (depends on 2)

The process of claim 2, wherein the filtration aid is a granulated substance having an average particle size of 150 μm or less.

### Claim 4 (depends on 3)

The process of claim 3, wherein the granulated substance is selected from the group consisting of diatomaceous earth, powdered cellulose and a combination thereof.

### Claim 5 (depends on 1)

The process of claim 1, wherein a metallic filter or a membrane filter is used as a filter medium in the filtration step.

### Claim 6 (depends on 1)

The process of claim 1, wherein the cellulose nanofibers are oxidized cellulose nanofibers.

### Claim 7 (depends on 1)

The process of claim 1, wherein the dispersion of cellulose nanofibers after the filtration has a contaminant area ratio of 25% or less when the amount of contaminants is evaluated by the following method:
1) forming a film after adding a surface tension adjustor to the dispersion of cellulose nanofibers after the filtration;
2) arranging a pair of polarizing plates on both sides of the film so that polarizing axes are orthogonalize with each other;
3) exposing light from one side of the polarizing plate, and obtaining a transmitted image from the other side of the polarizing plate; and
4) carrying out image analysis of the image to determine a contaminant area to calculate the contaminant area ratio per gram of bone dry weight of the cellulose nanofibers.

### Claim 8 (depends on 7)

The process of claim 7, wherein the dispersion of cellulose nanofibers after the filtration has the contaminant area ratio of 4% or less.

### Claim 9 (depends on 1)

A master batch prepared by the process of claim 1.

### Claim 10 (depends on 1)

A process for preparing a rubber composition, comprising:
the step of preparing the master batch by the method of claim 1; and
the step of crosslinking the master batch.

### Claim 11 (depends on 5)

The process of claim 5, wherein the cellulose nanofibers are oxidized cellulose nanofibers.

### Claim 12 (depends on 11)

The process of claim 11, wherein the dispersion of cellulose nanofibers after the filtration has a contaminant area ratio of 25% or less when the amount of contaminants is evaluated by the following method:
1) forming a film after adding a surface tension adjustor to the dispersion of cellulose nanofibers after the filtration;
2) arranging a pair of polarizing plates on both sides of the film so that polarizing axes are orthogonalize with each other;
3) exposing light from one side of the polarizing plate, and obtaining a transmitted image from the other side of the polarizing plate; and
4) carrying out image analysis of the image to determine a contaminant area to calculate the contaminant area ratio per gram of bone dry weight of the cellulose nanofibers.

### Claim 13 (depends on 12)

The process of claim 12, wherein the dispersion of cellulose nanofibers after the filtration has the contaminant area ratio of 4% or less.

### Claim 14 (depends on 8)

A master batch prepared by the process of claim 8.

### Claim 15 (depends on 8)

A process for preparing a rubber composition, comprising:
the step of preparing the master batch by the method of claim 8; and
the step of crosslinking the master batch.
