Surface-modified and dried microfibrillated cellulose reinforced thermoplastic biocomposites

Patent metadata

Field	Value
Publication number	US-12448512-B2
Application number	US-202117371581-A
Country	US
Kind code	B2
Filing date	Jul 9, 2021
Priority date	Jul 14, 2020
Publication date	Oct 21, 2025
Grant date	Oct 21, 2025

Abstract

A process for producing dried, vinyl carboxylate surface-modified microfibrillated cellulose having improved mechanical properties and a microfibril structure and a process for producing a vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester or thermoplastic polyolefin composite material having improved mechanical strength properties utilizing dried, vinyl carboxylate surface-modified microfibrillated cellulose.

First claim

What is claimed is:

1. A process for producing a vinyl-carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester or thermoplastic polyolefin biocomposite material having improved mechanical strength properties, the method comprising the following steps:
(a) preparing a dried, vinyl-carboxylate, surface-modified microfibrillated cellulose directly from pulp that is a water suspension of cellulose fibers by water-based surface modification of the suspended microfibrillated cellulose fibers including transesterification in the aqueous phase with water as the only solvent, and subsequent drying of the surface-modified microfibrillated cellulose;
(b) heating and mixing a thermoplastic polyester or thermoplastic polyolefin;
(c) combining the dried vinyl-carboxylate, surface-modified microfibrillated cellulose with the heated thermoplastic polyester or thermoplastic polyolefin in a mixing apparatus; and
(d) recovering the vinyl-carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester or thermoplastic polyolefin biocomposite; wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose thermoplastic polyester or thermoplastic polyolefin biocomposite demonstrates improved tensile strength and Young's modulus compared to neat thermoplastic polyester or thermoplastic polyolefin.

2. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl-carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 5 wt. %.

3. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 10 wt. %.

4. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 15 wt. %.

5. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl-carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 20 wt. %.

6. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl-carboxylate, surface-modified microfibrillated cellulose thermoplastic polyester biocomposite is about 25 wt. %.

7. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 30 wt. %.

8. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 40 wt. %.

9. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 50 wt. %.

10. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 30 wt. % to about 50 wt. %.

11. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 20 wt. % to about 50 wt. %.

12. The process according to claim 1 , wherein the vinyl-carboxylate, surface-modified microfibrillated cellulose content of the vinyl carboxylate, surface-modified microfibrillated cellulose-thermoplastic polyester biocomposite is about 20 wt. % to about 40 wt. %.

13. The process according to any one of claims 1 to 12 , wherein the vinyl carboxylate is vinyl laurate.

14. The process according to claim 1 , wherein the thermoplastic polyester is polylactic acid.

15. The process according to claim 1 , wherein the thermoplastic polyester is selected from the group consisting of polyglycolic acid (PGA), polylactic acid (PLA), polycaprolactone (PCL), polyhydroxyalkanoate (PHA), polyethylene adipate (PEA), and polyhydroxybutyrate (PHB), poly(lactic-co-glycolic acid (PLGA) and poly(lactic-co-glycolic acid)-poly-L-lysine (PLGA-PLL).

16. The process according to claim 1 , wherein the thermoplastic polyester is selected from the group consisting of polyethylene terephthalate (PET), polybutylene terephthalate (PBT), polytrimethylene terephthalate (PTT) and polyethylene naphthalate (PEN).

17. The process according to claim 16 , wherein the temperature in step (b) is about 80° C.

18. The process according to claim 1 , wherein the thermoplastic polyester is a polycondensation copolymer of 4-hydroxybenzoic acid and 6-hydroxynaphthalene-2-carboxylic acid (LCP) or a polyester of Bisphenol A and phthalic acid (PAR).

19. The process according to claim 1 , wherein the thermoplastic polyester is polybutylene succinate, or poly (3-hydroxybutyrate-co-3-hydroxyvalerate (PHBV).

20. The process according to claim 1 , wherein the thermoplastic polyester is an aliphatic polyester, aliphatic and semi-aromatic copolymers, or an aromatic copolymer.

21. The process according to claim 1 , wherein the thermoplastic polyolefin is selected from the group consisting of polyethylene (PE), polypropylene (PP), polymethylpentene (PMP), and polybutene-1 (PB-1).

22. The process according to claim 1 , wherein the thermoplastic polyolefin is selected from the group consisting of polyisobutylene (PIB), ethylene propylene rubber (EPR), and ethylene propylene diene monomer (M-class) rubber (EPDM rubber).

23. The process of any one of claims 1 to 12 , wherein the vinyl carboxylate is selected from the group of vinyl acetate, vinyl propionate, vinyl butyrate, vinyl valerate, vinyl pivalate, vinyl caproate, vinyl caprate, vinyl laurate, vinyl myristate, vinyl palmitate, vinyl stearate, vinyl cyclohexane carboxylate, vinyl octylate, vinyl methacrylate, vinyl crotonate, vinyl sorbate, vinyl benzoate, or vinyl cinamate, still more preferably vinyl acetate, vinyl propionate, vinyl butyrate, vinyl valerate, vinyl pivalate, vinyl caproate, vinyl caprate, vinyl laurate, vinyl myristate, vinyl palmitate, vinyl stearate, vinyl cyclohexane carboxylate, or vinyl octylate, and most preferably vinyl acetate, vinyl propionate, or vinyl butyrate.

24. The process according to claim 1 , further comprising the step of grinding the dried, vinyl-carboxylate, surface-modified microfibrillated cellulose.

Assignees

• Ut Battelle Llc
• Fiberlean Tech Ltd

Inventors

• Ozcan Soydan
• Li Kai
• Tekinalp Halil
• Zhao Xianhui
• Phipps Jon
• Ireland Sean

Classifications

• C08L2205/16

  Fibres; Fibrils · CPC title

• C08L1/10

  Esters of organic acids {, i.e. acylates} · CPC title

• C08B3/08

  of monobasic organic acids with three or more carbon atoms, {e.g. propionate or butyrate} · CPC title

• Y02E60/50

  Fuel cells · CPC title

• C08L67/04 Primary

  Polyesters derived from hydroxycarboxylic acids, e.g. lactones (C08L67/06 takes precedence) · CPC title