# US 10,246,583 B2 · Cellulose nanocrystal polymer composite

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- Number: US 10,246,583 B2
- Document ID: US10246583B2
- Status: Granted
- Kind: B2
- Application number: 15/315,550
- Filed: 2015-06-03
- Published: 2017-04-20
- Granted: 2019-04-02
- Earliest claimed: 2014-06-03
- Applicants: Blake Teipel; Elisa Teipel; Matt Kirby; Ryan Vano
- Inventors: Blake Teipel; Elisa Teipel; Matt Kirby; Ryan Vano
- Web page: https://patentgrep.com/patent/US10246583B2

## CPC

- C08L 63/00: Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08J 3/12: Powdering or granulating
- C08J 3/20: Compounding polymers with additives, e.g. colouring
- C08K 3/346: {Clay}
- C08K 5/19: Quaternary ammonium compounds
- C08L 1/04: Oxycellulose; Hydrocellulose {, e.g. microcrystalline cellulose}
- B29C 39/003: {characterised by the choice of material}
- B29K 2063/00: Use of {EP, i.e.} epoxy resins {or derivatives thereof}, as moulding material
- B29K 2105/162: {Nanoparticles}
- B29K 2201/00: Use of cellulose, modified cellulose or cellulose derivatives, e.g. viscose, as reinforcement
- C08J 2301/00: Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS

## Abstract

A reinforced polymer composite includes a polymer matrix and a strengthening agent. The strengthening agent includes highly crystalline cellulose nanocrystals (CNC) and a stabilizing agent. The crystalline cellulose nanocrystals (CNC) have dimensions of about 3 to 5 nm in width and about 100 to 300 nm in length and a density of about 1.6 g/cm3 and the stabilizing agent may be one of Boehmite nanoclay (Boe) and Cetyltrimethylammonium Bromide (CTAB) or a combination of both.

## Claims

### Claim 1

A reinforced polymer composite, the reinforced polymer composite comprising:
a polymer matrix, and
a strengthening agent, the strengthening agent including cellulose nanocrystals (CNC) and a stabilizing agent, wherein the stabilizing agent includes Boehmite nanoclay (Boe); and
wherein the strengthening agent is homogenously dispersed in the polymer matrix.

### Claim 2 (depends on 1)

The reinforced polymer composite of claim 1, wherein the cellulose nanocrystals (CNC) have dimensions of about 3 to 5 nm in width and about 100 to 300 nm in length.

### Claim 3 (depends on 1)

The reinforced polymer composite of claim 1, wherein the cellulose nanocrystals (CNC) are highly crystalline.

### Claim 4 (depends on 1)

The reinforced polymer composite of claim 1, wherein the cellulose nanocrystals (CNC) have a density of about 1.6 g/cm3.

### Claim 5 (depends on 1)

The reinforced polymer composite of claim 1 wherein the ratio of cellulose nanocrystals (CNC) to Boehmite nanoclay (Boe) is about 1 to 4.

### Claim 6 (depends on 1)

The reinforced polymer composite of claim 1 wherein the polymer matrix is a thermoset polymer matrix and the strengthening agent is added to the thermoset polymer matrix to achieve a mixture of about 2weight percent to about 10 weight percent strengthening agent.

### Claim 7

A reinforced polymer composite, the reinforced polymer composite comprising:
a polymer matrix, and
a strengthening agent, the strengthening agent including cellulose nanocrystals (CNC) and a stabilizing agent, wherein the stabilizing agent includes Cetyltrimethylammonium Bromide (CTAB) and wherein the ratio of cellulose nanocrystals (CNC) to Cetyltrimethylammonium Bromide (CTAB) is about 8 to 1; and
wherein the strengthening agent is homogenously dispersed in the polymer matrix.

### Claim 8 (depends on 7)

The reinforced polymer composite of claim 7 wherein the stabilizing agent further includes Boehmite nanoclay (Boe).

### Claim 9 (depends on 8)

The reinforced polymer composite of claim 8 wherein the ratio of cellulose nanocrystals (CNC) to Cetyltrimethylammonium Bromide (CTAB) to Boehmite nanoclay (Boe) is about 8 to 1 to 1.

### Claim 10

A method for preparing a reinforced polymer composite, the method including:
a first step includes providing an aqueous cellulose nanocrystal (CNC) suspension having a net negative charge;
a second step includes adding an appropriate amount of a stabilizer or a combination of stabilizers to the aqueous cellulose nanocrystal (CNC) suspension to achieve charge neutrality;
a third step includes inducing phase separation by processing the stabilized aqueous cellulose nanocrystal (CNC) suspension through at least one cycle of centrifugation, rinse, and redispersion;
a fourth step includes drying the stabilized cellulose nanocrystal (CNC) mixture;
a fifth step includes powderizing the dried stabilized cellulose nanocrystal (CNC) mixture; and
a sixth step includes adding the powderized dried stabilized cellulose nanocrystal (CNC) mixture to an uncured polymer prior to the addition of a hardener and cured.

### Claim 11 (depends on 10)

The method of preparing a reinforced polymer composite of claim 10, wherein the stabilizer is at least one of Boehmite nanoclay (Boe) and Cetyltrimethylammonium Bromide (CTAB).

### Claim 12 (depends on 10)

The method of preparing a reinforced polymer composite of claim 10, wherein drying the stabilized cellulose nanocrystal (CNC) mixture includes one of freeze drying, spray drying, and solvent drying the cellulose nanocrystal (CNC) mixture until a liquid solvent of the stabilized aqueous cellulose nanocrystal (CNC) suspension is sublimated.

### Claim 13 (depends on 10)

The method of preparing a reinforced polymer composite of claim 10, wherein rinsing the stabilized aqueous cellulose nanocrystal (CNC) suspension in the third step is performed with de-ionized water to remove any unbound stabilizer and maintain charge neutrality in the stabilized aqueous cellulose nanocrystal (CNC) suspension.

### Claim 14 (depends on 10)

The method of preparing a reinforced polymer composite of claim 10, wherein the first step further includes analyzing the aqueous cellulose nanocrystal (CNC) suspension using Dynamic Light Scattering (DLS) to determine the appropriate concentration of stabilizer to add in the second step.

### Claim 15

A reinforced polymer composite, the reinforced polymer composite comprising:
a polymer matrix, and
a strengthening agent, the strengthening agent including highly crystalline cellulose nanocrystals (CNC) and a stabilizing agent, and wherein the crystalline cellulose nanocrystals (CNC) have dimensions of about 3 to 5 nm in width and about 100 to 300 nm in length and a density of about 1.6 g/cm3 and the stabilizing agent includes Boehmite nanoclay (Boe) and Cetyltrimethylammonium Bromide (CTAB); and
wherein the strengthening agent is homogenously dispersed in the polymer matrix and is added to the polymer matrix to achieve a mixture of about 2 weight percent to about 10 weight percent strengthening agent.

### Claim 16 (depends on 15)

The reinforced polymer composite of claim 15, wherein the the ratio of cellulose nanocrystals (CNC) to Boehmite nanoclay (Boe) is about 1 to 4.

### Claim 17 (depends on 15)

The reinforced polymer composite of claim 15 wherein the ratio of cellulose nanocrystals (CNC) to Cetyltrimethylammonium Bromide (CTAB) is about 8 to 1.

### Claim 18 (depends on 15)

The reinforced polymer composite of claim 15 wherein the ratio of cellulose nanocrystals (CNC) to Cetyltrimethylammonium Bromide (CTAB) to Boehmite nanoclay (Boe) is about 8 to 1 to 1.