IP Library Granted Patent US 8,871,057
Granted Patent B2
US 8,871,057 · App. 13/138,647 · Granted Oct 28, 2014

Process for the production of nano-fibrillar cellulose suspensions

Inventors: Patrick A. C. Gane (Rothrist, CH); Joachim Schoelkopf (Killwangen, CH); Daniel Gantenbein (Basel, CH); Michel Schenker (Oftringen, CH); Michael Pohl (Villach, AT); Beat Kübler (Oberwil, CH)
Assignee: Omya International AG
D21B1/16D21C9/007D21D1/00D21H15/04D21H11/18
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Quick Facts
Patent No.
US 8,871,057
App. No.
13/138,647
Granted
Oct 28, 2014
Kind
B2
Abstract

The present invention relates to a process for the production of suspensions of nano-fibrillar cellulose 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 at least one filler and/or pigment, as well as the suspensions of nano-fibrillar cellulose obtained by this process and their uses.

Claims (60)

1. A process for the production of a nano-fibrillar cellulose suspension comprising the steps of:

(a) providing cellulose fibres;

(b) providing a filler;

(c) combining the cellulose fibres from step (a) and the filler from step (b); and

(d) fibrillating the cellulose fibres and the filler from step (c) to obtain a nano-fibrillar cellulose suspension,

wherein the filler is calcium carbonate, and wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:10 to 10:1.

2. The process according to claim 1 , wherein the cellulose fibres in step (a) are contained in pulps selected from eucalyptus pulp, spruce pulp, pine pulp, beech pulp, hemp pulp, cotton pulp, or any mixture thereof.

3. The process according to claim 1 , wherein the cellulose fibres in step (a) are contained in kraft pulp.

4. The process according to claim 1 , wherein the cellulose fibres in step (a) are contained in bleached longfibre kraft pulp.

5. The process according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension.

6. The process 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-%.

7. The process 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-%.

8. The process 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 5 wt-%.

9. The process 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 2 to 4.5 wt-%.

10. The process according to claim 1 , wherein the cellulose fibres in step (a) are provided in the form of a suspension at a solids content of about 1.3 or about 3.5 wt-%.

11. The process according to claim 1 , wherein the filler in step (b) is precipitated calcium carbonate.

12. The process according to claim 1 , wherein the filler in step (b) is precipitated calcium carbonate having a vateritic, a calcitic or an aragonitic crystal structure.

13. The process according to claim 1 , wherein the filler in step (b) is natural ground calcium carbonate.

14. The process according to claim 1 , wherein the filler in step (b) is natural ground calcium carbonate selected from marble, limestone and/or chalk.

15. The process according to claim 11 , wherein the precipitated calcium carbonate in step (b) is ultrafine discrete prismatic, scalenohedral or rhombohedral precipitated calcium carbonate.

16. The process according to claim 1 , wherein the filler in step (b) is in the form of particles having a median particle size of from 0.03 to 15 μm.

17. The process according to claim 1 , wherein the filler in step (b) is in the form of particles having a median particle size of from 0.2 to 5 μm.

18. The process according to claim 1 , wherein the filler in step (b) is in the form of particles having a median particle size of from 0.2 to 4 μm.

19. The process according to claim 1 , wherein the filler particles in step (b) is in the form of particles having a median particle size of about 1.5 or about 3.2 μm.

20. The process according to claim 1 , wherein the filler in step (b) comprises a dispersing agent.

21. The process according to claim 20 , 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- or tartaric acids, salts or esters thereof; or mixtures thereof.

22. The process according to claim 1 , wherein before fibrillating in step (d), the pH of the combination of the cellulose fibres and the filler is adjusted to a pH of 10 to 12.

23. The process according to claim 1 , wherein after fibrillating in step (d), the pH of the suspension is re-adjusted to a pH of 7.5 to 9.5.

24. The process according to claim 1 , wherein after fibrillating in step (d), the pH of the suspension is re-adjusted to a pH of about 8.5.

25. The process according to claim 1 , wherein the combination resulting from step (c) is stored for 2 to 12 hours prior to fibrillating in step (d).

26. The process according to claim 1 , wherein the combination resulting from step (c) is stored for 3 to 10 hours, prior to fibrillating in step (d).

27. The process according to claim 1 , wherein the combination resulting from step (c) is stored for 4 to 8 hours, prior to fibrillating in step (d).

28. The process according to claim 1 , wherein a cellulose solvent is added to the combination in step (c) prior to fibrillating in step (d).

29. The process according to claim 28 , wherein the cellulose solvent is copper(II)ethylenediamine, iron-sodium-tartrate or lithium-chloride/ dimethylacetamine.

30. The process according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:6 to 6:1.

31. The process according to claim 1 , wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:4 to 4:1.

32. The process 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.

33. The process 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.

34. The process according to claim 1 , wherein in step (d) 70 wt-% of bleached longfibre kraft pulp is fibrillated in the presence 30 wt-% ultrafine discrete prismatic or rhombohedral precipitated calcium carbonate (PCC), relative to the total dry weight of pulp and PCC, respectively.

35. The process according to claim 1 , wherein the combination from step (c) is fibrillated in step (d) until a Schopper Riegler degree is increased by ≧4°SR.

36. The process according to claim 1 , wherein the combination from step (c) is fibrillated in step (d) until a Schopper Riegler degree is increased by ≧6°SR.

37. The process according to claim 1 , wherein the combination from step (c) is fibrillated in step (d) until a Schopper Riegler degree is increased by ≧8°SR.

38. The process according to claim 1 , wherein the combination from step (c) is fibrillated in step (d) until a Schopper Riegler degree is increased by ≧10°SR.

39. The process according to claim 1 , wherein the combination from step (c) is fibrillated in step (d) until a Schopper Riegler degree is increased by ≧15°SR.

40. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧30°SR is reached.

41. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧45°SR is reached.

42. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧50°SR is reached.

43. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧60°SR is reached.

44. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧70°SR is reached.

45. The process according to claim 1 , wherein the combination of fibres and filler from step (c) is fibrillated in step (d) until a final Schopper-Riegler degree of ≧80°SR is reached.

46. The process according to claim 1 , wherein the fibrillating in step (d) is carried out by a device selected from an ultra-fine friction grinder, a refiner, or a homogenizer.

47. The process according to claim 1 , wherein the fibrillating in step (d) is carried out by an ultra-fine friction grinder or a homogenizer, and wherein the temperature of the suspension in the ultra-fine friction grinder or the homogenizer is above 60° C.

48. The process according to claim 1 , wherein the fibrillating in step (d) is carried out by an ultra-fine friction grinder or a homogenizer, and wherein the temperature of the suspension in the ultra-fine friction grinder or the homogenizer is above 80° C.

49. The process according to claim 1 , wherein the fibrillating in step (d) is carried out by an ultra-fine friction grinder or a homogenizer, and wherein the temperature of the suspension in the ultra-fine friction grinder or the homogenizer is above 90° C.

50. A process for the production of a nano-fibrillar cellulose suspension comprising the steps of:

(a) providing cellulose fibres;

(b) providing a filler;

(c) combining the cellulose fibres from step (a) and the filler from step (b); and

(d) fibrillating the cellulose fibres and the filler from step (c) to obtain a nano-fibrillar cellulose suspension,

wherein the filler comprises calcium carbonate and one or more of dolomite, talc, bentonite, clay, magnesite, satin white, sepiolite, huntite, diatomite, and a silicate, and wherein in step (d) the weight ratio of fibres to filler on a dry weight basis is from 1:10 to 10:1.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 21, 2016
From: OMYA INTERNATIONAL AG
To: OMYA-HOLDING AG
Reel/Frame 041119/0481 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 21, 2016
From: OMYA-HOLDING AG
To: FIBERLEANTM TECHNOLOGIES LIMITED
Reel/Frame 041119/0621 →
CHANGE OF NAME Recorded Nov 14, 2016
From: FIBERLEANTM TECHNOLOGIES LIMITED
To: FIBERLEAN TECHNOLOGIES LIMITED
Reel/Frame 040308/0951 →
CHANGE OF NAME Recorded Oct 14, 2013
From: OMYA DEVELOPMENT AG
To: OMYA INTERNATIONAL AG
Reel/Frame 031406/0917 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 14, 2011
From: GANE, PATRICK A; SCHOELKOPF, JOACHIM; GANTENBEIN, DANIEL; SCHENKER, MICHEL; POHL, MICHAEL; KUBLER, BEAT
To: OMYA DEVELOPMENT AG
Reel/Frame 027062/0975 →
Priority Claims (1)
EP 09156683 · Mar 30, 2009 · regional
Continuity (2)
Provisional Application 61212108 · Apr 6, 2009
Related Publication 20120094953A1 · Apr 19, 2012