IP Library Granted Patent US 8,975,318
Granted Patent B2
US 8,975,318 · App. 12/918,433 · Granted Mar 10, 2015

Halogen-free benzoxazine based curable compositions for high TG applications

Inventors: Roger Tietze (The Woodlands, TX); Yen-Loan Nguyen (Spring, TX)
Assignee: Huntsman Advanced Materials Americas LLC
C08K5/357C08G59/06C08G73/0233C08G59/24C08G59/4014C08G59/5046C08G59/621C08G59/683C08G2650/36C08L63/00C08L75/08
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Quick Facts
Patent No.
US 8,975,318
App. No.
12/918,433
Granted
Mar 10, 2015
Kind
B2
Abstract

The present invention provides a halogen-free curable composition including a benzoxazine monomer, at least one epoxy resin, a catalyst, a toughening agent and a solvent. The halogen-free curable composition is especially suited for use in automobile and aerospace applications since the composition, upon curing, produces a composite having a high glass transition temperature.

Claims (22)

1. A halogen-free curable composition comprising:

(a) a benzoxazine monomer of the formula (I)

wherein each R is, independently from one another, allyl, unsubstituted or substituted phenyl, unsubstituted or substituted C 1 -C 8 alkyl or unsubstituted or substituted C 3 -C 8 cycloalkyl;

(b) at least one epoxy resin;

(c) 5.7-10 parts by weight of a catalyst selected from tetraphenolethane;

(d) 5.7-10 parts by weigh of a toughening agent of the formula (II)

wherein m is 1 or 2, n is 2 to 6, R 0 is an n-valent radical of an elastomeric prepolymer after the removal of the terminal isocyanate, amino or hydroxyl groups, the elastomeric prepolymer being soluble or dispersible in epoxy resin, X and Y independently of one another are —O— or —NR 3 —, at least one X or Y being —NR 3 —, R 2 is an m+1-valent radical of polyphenol or aminophenol after the removal of the phenolic hydroxyl group(s) and optionally of the amino group, and R 3 is hydrogen, C 1 -C 6 alkyl or phenol; and

(e) a solvent

where the parts by weight are per 100 parts by weight of the composition.

2. The halogen-free curable composition according to claim 1 wherein R is phenyl.

3. The halogen-free curable composition according to claim 1 wherein the solvent is selected from the group consisting of methylethylketone, acetone, N-methyl-2-pyrrolidone, N,N-dimethyl formamide, pentanol, butanol, dioxolane, isopropanol, methoxy propanol, methoxy propanol acetate, dimethylformamide, glycol, glycol acetate, toluene, xylene and mixtures thereof.

4. A halogen-free curable composition comprising:

(a) 10-90 parts by weight of a benzoxazine monomer of the formula (I)

wherein each R is, independently from one another, allyl, unsubstituted or substituted phenyl, unsubstituted or substituted C 1 -C 8 -alkyl or unsubstituted or substituted C 3 -C 8 cycloalkyl;

(b) 2-60 parts by weight of at least one epoxy resin;

(c) 5.7-10 parts by weight of a catalyst selected from tetraphenolethane;

(d) 5.7-10 parts by weight of a toughening agent of the formula (II)

wherein m is 1 or 2, n is 2 to 6, R 0 is an n-valent radical of an elastomeric prepolymer after the removal of the terminal isocyanate, amino or hydroxyl groups, the elastomeric prepolymer being soluble or dispersible in epoxy resin, X and Y independently of one another are —O— or —NR 3 —, at least one X or Y being —NR 3 —, R 2 is an m+1-valent radical of polyphenol or aminophenol after the removal of the phenolic hydroxyl group(s) and optionally of the amino group, and R 3 is hydrogen, C 1 -C 6 alkyl or phenol; and

(e) 1-50 parts by weight of a solvent,

per 100 parts by weight of the halogen-free curable composition wherein the halogen-free curable composition, upon curing, has a glass transition temperature greater than 160° C.

5. The halogen-free curable composition according to claim 4 , wherein the glass transition temperature is greater than 200° C.

6. The halogen-free curable composition according to claim 4 , wherein the glass transition temperature is greater than 230° C.

Assignments (3)
CONFIRMATORY LICENSE Recorded Jun 15, 2018
From: GRAFTECH INTERNATIONAL
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 046098/0305 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 15, 2017
From: HUNTSMAN ADVANCED MATERIALS AMERICAS LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 042723/0477 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 26, 2010
From: TIETZE, ROGER; NGUYEN, YEN-LOAN
To: HUNTSMAN ADVANCED MATERIAL AMERICAS LLC
Reel/Frame 024891/0800 →
Continuity (2)
Provisional Application 61030366 · Feb 21, 2008
Related Publication 20100330287A1 · Dec 30, 2010