Analytical method for determining the concentration of oxidized nanofibrillar cellulose in a sample
US-2016299119-A1 · Oct 13, 2016 · US
US10294371B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10294371-B2 |
| Application number | US-201414474749-A |
| Country | US |
| Kind code | B2 |
| Filing date | Sep 2, 2014 |
| Priority date | Mar 30, 2009 |
| Publication date | May 21, 2019 |
| Grant date | May 21, 2019 |
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The present invention relates to a process for the production of nano-fibrillar cellulose gels by providing cellulose fibers and at least one filler and/or pigment; combining the cellulose fibers and the at least one filler and/or pigment; and fibrillating the cellulose fibers in the presence of the at least one filler and/or pigment until a gel is formed, as well as the nano-fibrillar cellulose gel obtained by this process and uses thereof.
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The invention claimed is: 1. A nano-fibrillar cellulose gel obtained by the process comprising the steps of: (a) providing cellulose fibres contained in pulps selected from the group consisting of eucalyptus pulp, spruce pulp, pine pulp, beech pulp, hemp pulp, cotton pulp, or any mixture thereof; (b) providing a filler; (c) combining the cellulose fibres of step (a) and the filler; and (d) fibrillating the cellulose fibres in an aqueous environment in the presence of the filler from step (c) until a nano-fibrillar cellulose gel is formed; wherein the formation of the gel is verified by monitoring the viscosity of the mixture in dependence of the shearing rate, wherein the viscosity decrease of the mixture upon step-wise increase of the shearing rate is stronger than the corresponding viscosity increase upon subsequent step-wise reduction of the shearing rate over at least part of the shear rate range as shearing approaches zero; wherein the filler is natural ground calcium carbonate, wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:33 to 10:1, wherein the Brookfield viscosity of the nano-fibrillar cellulose gel formed in step (d) is lower than the Brookfield viscosity of a corresponding nano-fibrillar cellulose suspension having been fibrillated in the absence of the filler. 2. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension. 3. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of from 0.2 to 35 wt.-%. 4. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of from 0.25 to 10 wt.-%. 5. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of from 0.5 to 5 wt.-%. 6. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of from 1 to 4 wt.-%. 7. The gel according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of from 1.3 to 3 wt.-%. 8. The gel according to claim 1 , wherein the filler in step (b) is natural ground calcium carbonate selected from marble, limestone and/or chalk. 9. The gel according to claim 1 , wherein the filler in step (b) is in the form of particles having a median medium particle size of from 0.01 to 15 μm. 10. The gel according to claim 1 , wherein the filler in step (b) is in the form of particles having a median medium particle size of from 0.1 to 10 μm. 11. The gel according to claim 1 , wherein the filler in step (b) is in the form of particles having a median medium particle size of from 0.3 to 5 μm. 12. The gel according to claim 1 , wherein the filler in step (b) is in the form of particles having a median medium particle size of from 0.5 to 4 μm. 13. The gel according to claim 1 , wherein the filler in step (b) comprises a dispersing agent. 14. The gel according to claim 13 , wherein the dispersing agent is selected from homopolymers or copolymers of polycarboxylic acids and/or their salts or esters, acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, acryl amide or acrylic esters, or mixtures thereof; alkali polyphosphates, phosphonic-, citric- and tartaric acids, salts or esters thereof; or mixtures thereof. 15. The gel according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:10 to 7:1. 16. The gel according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:5 to 5:1. 17. The gel according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:3 to 3:1. 18. The gel according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:2 to 2:1. 19. The gel according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:1.5 to 1.5:1. 20. The gel according to claim 1 , wherein the fibrillating in step (d) is carried out by a homogenizer or an ultra fine friction grinder. 21. A material composite, plastic, paint, rubber, concrete, ceramic, adhesive, food or wound-healing composite comprising the nano-fibrillar cellulose gel according to claim 1 .
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