Microfibrillated cellulose and method for preparing a microfibrillated cellulose

• US 5,964,983 A
• Filed: 07/16/1997
• Issued: 10/12/1999
• Est. Priority Date: 02/08/1995
• Status: Expired due to Fees

• Current Assignee: Generale Sucriere
• Original Assignee: General Sucriere
• Inventors: Vignon, Michel R., Maureaux, Alain, Dinand, Elisabeth, Chanzy, Henri, Vincent, Isabelle
• Primary Examiner(s): NGUYEN, TAN D
• Application Number:
  US08/875,028
• Time in Patent Office: 818 Days
• Field of Search: 162/26, 162/27, 162/76, 162/182, 162/158, 162/173, 162/187, 426/94, 426/572, 426/573, 426/659
• US Class Current: 162/27
• CPC Class Codes: C09K 8/206 Derivatives of other natural products, e.g. cellulose, starch, sugars
• CPC Class Codes: D21C 5/00 Other processes for obtaining cellulose, e.g. cooking cotton linters obtaining fibres for spinning D01C; Processes characterised by the choice of cellulose-containing starting materials
• CPC Class Codes: D21H 11/12 Pulp from non-woody plants or crops, e.g. cotton, flax, straw, bagasse
• CPC Class Codes: D21H 11/18 Highly hydrated, swollen or fibrillatable fibres

Abstract

A microfibrillated cellulose containing at least around 80% of primary walls and loaded with carboxylic acids, and a method for preparing same, in particular from sugar beet pulp, wherein the pulp is hydrolysed at a moderate temperature of 60-100° C.; at least one extraction of the cellulose material is performed using a base having a concentration of less than 9 wt. %; and the cellulose residue is homogenised by mixing, grinding or any high mechanical shear processing, whereafter the cell suspension is fed through a small-diameter aperture, and the suspension is subjected to a pressure drop of at least 20 MPa and high-speed sheer action followed by a high-speed deceleration impact. The cellulose is remarkable in that a suspension thereof can easily be recreated after it has been dehydrated.

Claims

1. A microfibrillated cellulose containing at least 80% of primary walls and wherein the primary walls are charged with or contain uronic acids.

2. The microfibrillated cellulose according to claim 1 containing at least about 85% of primary walls.

3. The microfibrillated cellulose according to claim 1 wherein the uronic acids are selected from the group consisting of galacturonic acid and glucuronic acid.

4. The microfibrillated cellulose according to claim 1 wherein the cellulose has a crystallinity of 15% to 50%.

5. The microfibrillated cellulose according to claim 1 wherein the cellulose comprises microfibrils with a cross-section between about 2 nm and about 4 nm.

6. A process for the preparation of microfibrillated cellulose from primary wall plant pulp containing cellulose, pectins, hemicelluloses, proteins and mineral materials, the process comprising the following steps:

(a) hydrolyzing the pulp with acid or base at a temperature between about 60°

C. and 100°

C. partially to extract the pectins and hemicelluloses to form a suspension;

(b) recovering a solid residue from the suspension from step (a);

(c) carrying out, under alkaline conditions, a second extraction of the residue of cellulosic material from step (b), when step (a) is an acidic hydrolysis and

recovering the cellulosic material residue by separating the suspension;

(d) washing the residue from step (b) or step (c);

(e) diluting the cellulosic material from step (d) in water to obtain between 2% and 10% dry matter;

(f) homogenizing the cell suspension from step (e) wherein

at least one alkaline extraction step is carried out on the cellulosic material, said alkaline extraction being carried out with a base at a concentration less than about 9% by weight, and

the homogenizing step (f) is carried out by a high mechanical shear operation to provide a cell suspension, passing the cell suspension through a small diameter orifice, subjecting the suspension to a pressure drop of at least 20 MPa and to a high velocity shearing action followed by a high velocity decelerating impact.

7. A process according to claim 6 wherein step (a) hydrolysis is at a temperature between about 70°

C. and 95°

C.

8. A process according to claim 7, wherein step (a) hydrolysis is at a temperature of about 90°

C.

9. A process according to claim 6 wherein in each alkaline extraction step a base selected from the group consisting of caustic soda and potash is used.

10. A process according to claim 6 wherein the concentration of the base used for each alkaline extraction step is in the range from about 1% to about 6% by weight.

11. A process according to claim 6 wherein an additive selected from the group consisting of dispersing agents, suspending agents and thickening agents which are soluble in water is added to the suspension to be homogenized in step (f).

12. A process according to claim 6 wherein the homogenization step (f) is at a temperature between 95°

C. and 120°

C.

13. A process according to claim 6, wherein before step (a), the dehydrated pulp is ground and screened and retaining the fraction with a granulometry between about 20 μ

m and about 1,000 μ

m.

14. A process according to claim 6 wherein after washing step (d) or after bleaching the cellulosic suspension is moderately ground wet followed by filtering with a screen mesh between about 20 μ

m and about 75 μ

m.

15. A process according to claim 6, wherein cellulose resulting from homogenization step (f) is concentrated.

16. A process according to claim 15 wherein the cellulose is concentrated to more than about 50% dry matter.

17. A process according to claim 15 wherein the cellulose is concentrated by pressing, filtering or low temperature and controlled humidity drying.

18. A process according to claim 6 wherein the homogenization of step (f) is followed by a high shear operation.

19. A process according to claim 6 wherein the plant pulp is saccharose-extracted beet pulp.

20. A process according to claim 6 including the step of bleaching the cellulosic material after step (d) to provide a suspension of cellulosic material and recovering the cellulosic material by separating said cellulosic material from the suspension.

21. A process according to claim 20 wherein the material is bleached with an oxidizing treatment with ozone or hydrogen peroxide.

22. A process according to claim 21 wherein the ozone or hydrogen peroxide is used in the bleaching.

23. A process according to claim 6, wherein the dehydrated pulp is ground and screened and retaining the fraction with a granulometry between about 75 μ

m and 600 μ

m.

24. A process according to claim 6 wherein the high-shear operation is mixing or grinding.