IP Library Granted Patent US 10,626,226
Granted Patent B2
US 10,626,226 · App. 15/739,369 · Granted Apr 21, 2020

Synthetically modified thermoplastic polymer composites having cellulose nanomaterials

Inventors: Blake Teipel (College Station, TX); Elisa Teipel (College Station, TX); Matt Kirby (College Station, TX); Ryan Vano (College Station, TX); Mustafa Akbulut (College Station, TX)
Assignee: Essentium Inc.
C08J3/126B82Y30/00C08F120/08C08L1/02C08L33/00C09D123/26C08F2500/24C08J2300/22C08L2205/16C08L2205/18C08L2207/53
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Quick Facts
Patent No.
US 10,626,226
App. No.
15/739,369
Granted
Apr 21, 2020
Kind
B2
Abstract

A method of manufacturing a polymer coated cellulose nanocrystal composite material begins with an aqueous cellulose nanocrystal (CNC) suspension mixture. The aqueous CNC suspension mixture is dried to remove the liquid solvent from the aqueous CNC suspension mixture to form a dry CNC powder. Diethylenetriamine (DETA) is combined with melted Maleated-anhydride Polypropylene (MAPP) to form a DETA-functionalized MAPP (MA) mixture. The MA mixture is cooled and pelletized to form MA pellets. The MA pellets, the dry CNC powder, and a neat polypropylene (PP) are combined to form a CNC-PP mixture. The CNC-PP mixture is compounded by melting, subsequently cooled and pelletized to form CNC-PP pellets.

Claims (27)

1. A method of manufacturing a polymer coated cellulose nanocrystal composite material, the method comprising:

providing an aqueous cellulose nanocrystal (CNC) suspension mixture;

drying the aqueous CNC suspension mixture to remove the liquid solvent from the aqueous CNC suspension mixture to form a dry CNC powder;

combining an Amine to melted Maleated-anhydride Polypropylene (MAPP) to form an Amine-functionalized MAPP (MA) mixture at a weight percent ratio of Maleic acid (MAH):NH 2 of between 2:1 to 1:3;

cooling and pelletizing the MA mixture to form MA pellets;

combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture;

compounding the CNC-PP mixture by melting, and

cooling and pelletizing the CNC-PP mixture to form CNC-PP pellets.

2. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein drying the aqueous CNC suspension mixture to remove the liquid solvent from the aqueous CNC suspension mixture to form a dry CNC powder further comprises drying the aqueous CNC suspension mixture to remove the liquid solvent from the aqueous CNC suspension mixture to form a dry CNC powder by at least one of freeze drying, spray drying, and solvent drying the aqueous CNC suspension mixture.

3. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture further comprises combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture wherein combining the MA pellets and the dry CNC powder is at a weight percent ratio CNC:MA of between 1:2 to 1:19.

4. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein compounding the CNC-PP mixture by melting further comprises compounding the CNC-PP mixture by melting in a high shear environment.

5. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein providing an aqueous cellulose nanocrystal (CNC) suspension mixture further comprises providing an aqueous cellulose nanocrystal (CNC) suspension mixture wherein a CNC of the CNC suspension mixture is highly crystalline, has a rectangular shape, and has a density of about 1.6 g/cm 3 .

6. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein providing an aqueous cellulose nanocrystal (CNC) suspension mixture further comprises providing an aqueous cellulose nanocrystal (CNC) suspension mixture suspension mixture wherein a CNC of the CNC suspension mixture is thermally stable in a nitrogen environment up to 250° C., in an atmospheric environment up to 230° C. and has a strong negative surface charge of −45±1.8 mV.

7. The method of manufacturing a polymer coated cellulose nanocrystal of claim 1 , wherein combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture further comprises combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture wherein the MA pellets and the dry CNC powder are at a weight percent ratio CNC:MA of between about 1:5 to about 1:10.

8. A method of manufacturing a polymer coated cellulose nanocrystal composite material, the method comprising:

providing an aqueous cellulose nanocrystal (CNC) suspension mixture;

drying the aqueous CNC suspension mixture to remove the liquid solvent from the aqueous CNC suspension mixture to form a dry CNC powder using at least one of freeze drying, spray drying, and solvent drying, and wherein a CNC of the dry CNC powder is highly crystalline and has a rectangular shape;

combining an Amine to melted Maleated-anhydride Polypropylene (MAPP) to form an Amine-functionalized MAPP (MA) mixture at a weight percent ratio of Maleic acid (MAH):NH 2 of between 2:1 to 1:3;

cooling and pelletizing the MA mixture to form MA pellets;

combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture;

compounding the CNC-PP mixture by melting, and

cooling and pelletizing the CNC-PP mixture to form CNC-PP pellets.

9. The method of manufacturing a polymer coated cellulose nanocrystal of claim 8 , wherein combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture further comprises combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture wherein combining the MA pellets and the dry CNC powder is at a weight percent ratio CNC:MA of between 1:2 to 1:19.

10. The method of manufacturing a polymer coated cellulose nanocrystal of claim 9 , wherein compounding the CNC-PP mixture by melting further comprises compounding the CNC-PP mixture by melting in a high shear environment.

11. The method of manufacturing a polymer coated cellulose nanocrystal of claim 10 , wherein providing an aqueous cellulose nanocrystal (CNC) suspension mixture further comprises providing an aqueous cellulose nanocrystal (CNC) suspension mixture wherein a CNC of the CNC suspension mixture has a density of about 1.6 g/cm3.

12. The method of manufacturing a polymer coated cellulose nanocrystal of claim 11 , wherein providing an aqueous cellulose nanocrystal (CNC) suspension mixture further comprises providing an aqueous cellulose nanocrystal (CNC) suspension mixture wherein the CNC of the CNC suspension mixture is thermally stable in a nitrogen environment up to 250° C., in an atmospheric environment up to 230° C. and has a strong negative surface charge of −45±1.8 mV.

13. The method of manufacturing a polymer coated cellulose nanocrystal of claim 12 , wherein combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture further comprises combining the MA pellets, the dry CNC powder, and a neat polypropylene (PP) to form a CNC-PP mixture wherein the MA pellets and the dry CNC powder are at a weight percent ratio CNC:MA of between about 1:5 to about 1:10.

Assignments (12)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 17, 2025
From: NEXA3D INC.; NXT FACTORY, INC.
To: STRATASYS, INC.
Reel/Frame 071657/0111 →
RELEASE OF SECURITY INTEREST Recorded Jun 10, 2025
From: U.S. BANK TRUST COMPANY
To: NEXA3D INC.; NXT FACTORY INC.; NEXA3D APS
Reel/Frame 071534/0581 →
SECURITY INTEREST Recorded Nov 15, 2024
From: NEXA3D INC.; NXT FACTORY INC.; NEXA3D APS
To: U.S. BANK TRUST COMPANY
Reel/Frame 069381/0694 →
RELEASE OF SECURITY INTEREST Recorded Jan 17, 2024
From: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION
To: ESSENTIUM, INC.; ESSENTIUM IPHOLDCO, LLC; ESSENTIUM IPCO, LLC
Reel/Frame 066339/0087 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 17, 2024
From: ESSENTIUM IPCO, LLC.
To: NEXA3D INC.
Reel/Frame 066339/0185 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 16, 2022
From: ESSENTIUM, INC.
To: ESSENTIUM IPCO, LLC
Reel/Frame 061950/0803 →
RELEASE OF SECURITY INTEREST Recorded Jul 18, 2022
From: SILICON VALLEY BANK
To: ESSENTIUM, INC.
Reel/Frame 060682/0613 →
SECURITY INTEREST Recorded Jun 27, 2022
From: ESSENTIUM, INC.; ESSENTIUM IPHOLDCO, LLC; ESSENTIUM IPCO, LLC
To: U.S. BANK TRUST COMPANY, NATIONAL ASSOCIATION, AS THE COLLATERAL AGENT
Reel/Frame 060445/0808 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 13, 2022
From: KIRBY, MATT
To: ESSENTIUM, INC.
Reel/Frame 058647/0388 →
SECURITY INTEREST Recorded Sep 20, 2021
From: ESSENTIUM, INC.
To: QSHGP, INC.
Reel/Frame 057545/0005 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 22, 2021
From: TEIPEL, BLAKE; TEIPEL, ELISA; AKBULUT, MUSTAFA; VANO, RYAN
To: ESSENTIUM, INC.
Reel/Frame 055666/0379 →
SECURITY INTEREST Recorded Oct 27, 2020
From: ESSENTIUM, INC.
To: SILICON VALLEY BANK
Reel/Frame 054198/0663 →