# US 9,751,969 B2 · NCC-based supramolecular materials for thermoplastic and thermoset polymer composites

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- Number: US 9,751,969 B2
- Document ID: US9751969B2
- Status: Granted
- Kind: B2
- Application number: 14/344,797
- Filed: 2012-09-12
- Published: 2014-11-27
- Granted: 2017-09-05
- Earliest claimed: 2011-09-13
- Assignees: Celluforce Inc.
- Applicants: Wadood Y. Hamad; Shunxing Su
- Inventors: Wadood Y. Hamad; Shunxing Su
- Web page: https://patentgrep.com/patent/US9751969B2

## CPC

- C08F 251/02: on to cellulose or derivatives thereof
- C08L 23/06: Polyethylene
- C08L 51/02: grafted on to polysaccharides
- C08L 1/02: Cellulose; Modified cellulose
- C08L 2207/04: Thermoplastic elastomer
- C08L 2207/062: HDPE
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)

## Abstract

Nanocrystalline cellulose (NCC)-based supramolecular materials, a method for their preparation and their use in thermoplastic and thermoset polymer composites are disclosed. Supramolecular materials of NCC and one or two polymers are synthesized by in situ surface graft copohmerization in a multitude of solvent systems, including water. The nano-scale size supramolecular materials are engineered to have a unique combination of lower polarity and high hydrophobicity and function as copohmers for demanding pohmeric systems such as, but not limited to, polyolefins and polyesters. Nanocomposite materials of enhanced functionality and mechanical properties are produced by compounding the NCC-based supramolecular materials with polymer matrices. The supramolecular materials are used in composite development for packaging materials, structural composites for automotive and construction, as sandwiched foam composites or, combined with biocompatible polymers, in medical applications.

## Claims

### Claim 1

A process for preparing NCC-based supramolecular material comprising:
(i) providing a mixture comprising Na-NCC or a surfactant-modified-NCC and one or more water-insoluble monomer(s) in an organic solvent, said mixture being suitable for free radical polymerization, and wherein said one or more water-insoluble monomer(s) comprises a methacrylate or acrylate monomer;
(ii) providing a solution of a free radical initiator in an organic solvent;
(iii) purging oxygen from the mixture of (i) and the solution of (ii);
(iv) mixing (i) and (ii) after step (iii) and polymerizing said water-insoluble monomer(s) in said organic solvent; and
(v) isolating said NCC-based supramolecular material.

### Claim 2 (depends on 1)

The process of claim 1, wherein said mixture in step (i) is a mixture of Na-NCC and one or more water-insoluble monomer(s) in an organic solvent.

### Claim 3 (depends on 1)

The process of claim 1, wherein said mixture in step (i) is a mixture of a surfactant-modified-NCC and one or more water-insoluble monomer(s) in an organic solvent.

### Claim 4 (depends on 1)

The process of claim 1, wherein said one or more water-insoluble monomer is a lipophilic aliphatic chains-containing methacrylate or acrylate ester.

### Claim 5 (depends on 4)

The process of claim 4, wherein said aliphatic chain-containing methacrylate or acrylate ester is comprising 8 or more carbon atoms in said aliphatic chain.

### Claim 6 (depends on 3)

The process of claim 3, wherein the surfactant of said surfactant-modified-NCC is a cationic surfactant.

### Claim 7 (depends on 6)

The process of claim 6, wherein said cationic surfactant is a quaternary ammonium surfactant.

### Claim 8 (depends on 4)

The process of claim 4, wherein said aliphatic chain-containing methacrylate or acrylate esters is comprising 8 to 20 carbon atoms.

### Claim 9 (depends on 1)

The process of claim 1, wherein said one or more water-insoluble monomer(s) comprises octyl methacrylate, lauryl methacrylate, dodecyl acrylate, hexadecyl acrylate, hexadecyl methacrylate, stearyl methacrylate or a mixture thereof.

### Claim 10 (depends on 7)

The process of claim 7, wherein said quaternary ammonium surfactant is cetyl trimethylammonium bromide (CTAB), cetyl trimethylammonium chloride (CTAC), Cetylpyridinium chloride (CPC), Benzalkonium chloride (BAC), Benzethonium chloride (BZT), Dimethyldioctadecylammonium chloride or Dioctadecyldimethylammonium bromide (DODAB).