# US 11,111,379 B2 · Polymer nanocomposite comprising poly(ethylene terephthalate) reinforced with an intercalated phyllosilicate

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- Number: US 11,111,379 B2
- Document ID: US11111379B2
- Status: Granted
- Kind: B2
- Application number: 16/331,471
- Filed: 2017-09-14
- Published: 2019-07-18
- Granted: 2021-09-07
- Earliest claimed: 2016-09-15
- Assignees: Instituto TecnolóGico Del Embalaje, Transporte Y LogíStica (Itene)
- Applicants: Instituto TecnolóGico Del Embalaje, Transporte Y LogíStica (Itene)
- Inventors: María Jordá Beneyto; Natalia Ortuño Mansilla; Maria Del Carmen Sánchez Reig; Miriam Gallur Blanca; Susana Aucejo Romero; Javier Zabaleta Meri
- Web page: https://patentgrep.com/patent/US11111379B2

## CPC

- C08L 67/02: Polyesters derived from dicarboxylic acids and dihydroxy compounds (C08L67/06 takes precedence)
- B29C 49/0005: {characterised by the material}
- C08G 63/16: Dicarboxylic acids and dihydroxy compounds
- C08G 63/181: Acids containing aromatic rings
- C08J 3/226: {using a polymer as a carrier}
- C08J 5/005: {Reinforced macromolecular compounds with nanosized materials, e.g. nanoparticles, nanofibres, nanotubes, nanowires, nanorods or nanolayered materials}
- C08K 3/346: {Clay}
- C08K 5/19: Quaternary ammonium compounds
- C08K 9/08: Ingredients agglomerated by treatment with a binding agent
- C08K 13/02: Organic and inorganic ingredients
- B29C 49/06: Injection blow-moulding
- B29C 2949/0715: the preform having one end closed
- B29K 2067/003: {PET, i.e. poylethylene terephthalate}
- B29K 2105/162: {Nanoparticles}
- B29K 2509/00: Use of inorganic materials not provided for in groups {B29K2503/00 - B29K2507/00,} as filler
- B29L 2031/7158: {Bottles}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C08J 2367/02: Polyesters derived from dicarboxylic acids and dihydroxy compounds; (C08J2367/06 takes precedence)
- C08K 2201/008: Additives improving gas barrier properties
- C08K 2201/011: Nanostructured additives
- C08L 2201/14: Gas barrier composition
- C08L 2203/10: used for bottles
- C08L 2205/025: containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
- C08L 2310/00: Masterbatches
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- 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)
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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)
- 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
- B29L: INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

It is provided a phyllosilicate having a layered structure in the form of platelets and comprising an intercalating agent between the platelets, wherein the intercalating agent is a polyester of a molecular weight of 274 to 30,000 g/mol, and wherein the phyllosilicate is other than a phyllosilicate modified through ionic interchange. It is also provides a polymer nanocomposite comprising a polyethylene terephthalate (PET) polymer an the phyllosilicate mentioned above, as well as preparation processes for the preparation of the intercalated phyllosilicate and the PET nanocomposite. The PET nanocomposite is particularly useful for packaging, particularly for food and drink packaging.

## Claims

### Claim 1

An intercalated phyllosilicate having a structure of layers and comprising an intercalating agent between the layers, wherein the intercalating agent is a polyester of a molecular weight of 274 to 30,000 g/mol selected from polyadipate, polyphthalate, and a mixture thereof, and wherein the phyllosilicate is other than a phyllosilicate modified through ionic interchange.

### Claim 2 (depends on 1)

The intercalated phyllosilicate according to claim 1, wherein the weight ratio of intercalating agent to phyllosilicate is 5:95 to 60:40.

### Claim 3 (depends on 1)

The intercalated phyllosilicate according to claim 1, wherein the polyester is polyadipate.

### Claim 4 (depends on 1)

The intercalated phyllosilicate according to claim 1, wherein the polyester has a molecular weight of 1,000 to 5,000 g/mol.

### Claim 5 (depends on 1)

The intercalated phyllosilicate according to claim 1, wherein the phyllosilicate is selected from the group consisting of a montmorillonite, sepiolite, halloysite, bentonite, kaolinite, wollastonite, and mica.

### Claim 6 (depends on 1)

The intercalated phyllosilicate according to claim 1, wherein the phyllosilicate is selected from the group consisting of sodium montmorillonite, magnesium montmorillonite, and calcium montmorillonite.

### Claim 7 (depends on 6)

The intercalated phyllosilicate according to claim 6, wherein the phyllosilicate is sodium montmorillonite.

### Claim 8 (depends on 1)

A polymer nanocomposite comprising:
a polyethylene terephthalate (PET) polymer; and
an intercalated phyllosilicate as defined in claim 1.

### Claim 9 (depends on 8)

The polymer nanocomposite according to claim 8, wherein the weight-to-weight ratio of intercalated phyllosilicate to PET polymer is from 0.2:99.8 to 20:80.

### Claim 10 (depends on 1)

A process for the preparation of the intercalated phyllosilicate as defined in claim 1 comprising:
i) dispersing a phyllosillicate which is other than a phyllosilicate modified through ionic interchange in a solvent selected from water and a mixture of water and a C1-C10 alcohol under stirring;
ii) optionally, submitting the dispersion to ultrasonic treatment;
iii) mixing the dispersion with an intercalating agent selected from polyadipate, polyphthalate, and a mixture thereof, optionally in a mixture of water and a C1-C10 alcohol;
iv) keeping the mixture of step iii) under continuous stirring for 17 to 24 hours at a temperature from 60° C. to 75° C.; and
v) isolating the compound obtained in step (iv).

### Claim 11 (depends on 1)

A process for the preparation of a PET nanocomposite, the process comprising melt-blending a PET polymer and the intercalated phyllosillicate as defined in claim 1.

### Claim 12 (depends on 1)

A method for reinforcing a polyethylene terephthalate (PET) polymer comprising incorporating into the PET polymer an intercalated phyllosilicate as defined in claim 1.

### Claim 13 (depends on 8)

An article of manufacture made of the polymer nanocomposite as defined in claim 8.

### Claim 14 (depends on 8)

A process for the preparation of an article of manufacture made of the polymer nanocomposite as defined in claim 8, the process comprising:
a) dispersing a phyllosilicate which is other than a phyllosilicate modified through ionic interchange in an intercalating agent;
b) mixing the dispersion obtained in step a) with the PET polymer; and
c) obtaining an article of manufacture by extrusion, injection or injection stretch blow moulding of the mixture obtained in step b);
wherein the intercalating agent is a polyester of a molecular weight of 274 to 30,000 g/mol, and wherein the phyllosilicate is not modified through ionic interchange.

### Claim 15 (depends on 2)

The intercalated phyllosilicate according to claim 2, wherein the polyester is polyadipate.

### Claim 16 (depends on 15)

The intercalated phyllosilicate according to claim 15, wherein the polyester has a molecular weight of 1,000 to 5,000 g/mol.

### Claim 17

The intercalated phyllosilicate according to 16, wherein the phyllosilicate is selected from the group consisting of sodium montmorillonite, magnesium montmorillonite, and calcium montmorillonite.

### Claim 18 (depends on 17)

A polymer nanocomposite comprising:
a polyethylene terephthalate (PET) polymer; and
an intercalated phyllosilicate as defined in claim 17.

### Claim 19 (depends on 18)

The polymer nanocomposite according to claim 18, wherein the weight-to-weight ratio of the intercalated phyllosilicate to PET polymer is from 0.2:99.8 to 20:80.

### Claim 20 (depends on 19)

An article of manufacture made of the polymer nanocomposite as defined in claim 19.