IP Library Granted Patent US 9,365,750
Granted Patent B2
US 9,365,750 · App. 13/785,336 · Granted Jun 14, 2016

Accelerators for curable compositions

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Quick Facts
Patent No.
US 9,365,750
App. No.
13/785,336
Granted
Jun 14, 2016
Kind
B2
Abstract

Benzoylthiourea or benzoylthiourethane derivatives as cure accelerators for curable compositions are provided.

Claims (27)

1. An anaerobic curable composition, comprising:

(a) a (meth)acrylate component;

(b) an anaerobic cure-inducing composition comprising a peroxide and a benzoyl thiourea or benzoyl thiourethane compound as an anaerobic cure accelerator within structures I or IA below:

wherein Z is O or N—R, where R is selected from hydrogen, alkyl, alkenyl, aryl, hydroxyalkyl, hydroxyalkenyl, alkylene (meth)acrylate, carbonyl, carboxyl, or sulfonato, and R′ taken together form a carbocyclic or hetero atom-containing ring, or R′ is a direct bond attaching to the phenyl ring; X is optional, but when present is halogen, alkyl, alkenyl, cycloalkyl, hydroxyalkyl, hydroxyalkenyl, alkoxy, amino, alkylene- or alkenylene-ether, alkylene(meth)acrylate, carbonyl, carboxyl, nitroso, sulfonate, hydroxyl or haloalkyl; and Y is —SO 2 NH—, —CONH—, —NH—, and —PO(NHCONHCSNH 2 )NH—; and n is 0 or 1 and m is 1 or 2;

wherein R and R′ are independently selected from hydrogen, alkyl, alkenyl, aryl, hydroxyalkyl, hydroxyalkenyl, alkylene (meth)acrylate, carbonyl, carboxyl, or sulfonato, or R and R′ taken together form a carbocyclic or hetero atom-containing ring, or R′ is a direct bond attaching to the phenyl ring; X is optional, but when present is halogen, alkyl, alkenyl, cycloalkyl, hydroxyalkyl, hydroxyalkenyl, alkoxy, amino, alkylene- or alkenylene-ether, alkylene(meth)acrylate, carbonyl, carboxyl, nitroso, sulfonate, hydroxyl or haloalkyl; and Y is —SO 2 NH—, —CONH—, —NH—, and —PO(NHCONHCSNH 2 )NH—; and n is 0 or 1 and m is 1 or 2.

2. The composition of claim 1 , wherein the anaerobic cure accelerator is within structure II or IIA below:

wherein R, R′, X, Y, and n are as defined above.

3. The composition of claim 1 , wherein the anaerobic cure accelerator is within structure III or IV below:

wherein R, X, Y, and n are as defined above, and X′ is defined as X.

4. The composition according to claim 1 , wherein the (meth)acrylate component is represented by H 2 C═CGCO 2 R 1 , wherein G is a member selected from the group consisting of H and alkyl having from 1 to about four carbon atoms, and R 1 is a member selected from the group consisting of alkyl, cycloalkyl, alkenyl, cycloalkenyl, alkaryl, and aryl groups having from 1 to about 16 carbon atoms, with or without substitution or interruption by a member selected from the group consisting of silane, silicon, oxygen, halogen, carbonyl, hydroxyl, ester, carboxylic acid, urea, urethane, carbamate, amine, amide, sulfur, sulfonate and sulfone.

5. The composition according to claim 1 , wherein the (meth)acrylate component is a member selected from the group consisting of silicone (meth)acrylates, polyethylene glycol di(meth)acrylates, bisphenol-A-(meth)acrylates, ethoxylated bisphenol-A-(meth)acrylates, bisphenol-F-(meth)acrylates, ethoxylated bisphenol-F-(meth)acrylates, tetrahydrofuran(meth)acrylates and di(meth)acrylates, hydroxypropyl(meth)acrylate, hexanediol di(meth)acrylate, and trimethylol propane tri(meth)acrylate.

6. The composition according to claim 1 , further comprising an additional accelerator.

7. The composition according to claim 6 , wherein the additional accelerator is saccharin.

8. Reaction products of the composition according to claim 1 .

9. A process for preparing a reaction product from an anaerobic curable composition, comprising the steps of:

apply an anaerobic curable composition according to claim 1 , to a desired substrate surface and

exposing the composition to an anaerobic environment for a time sufficient to cure the composition.

10. A method of preparing an anaerobic curable composition, comprising the step of:

mixing together:

a (meth)acrylate component,

an anaerobic cure inducing composition and

as an anaerobic cure accelerator a benzoyl thiourea or benzoyl thiourethane compound within structures I or IA

wherein R and R′ are independently selected from hydrogen, alkyl, alkenyl, aryl, hydroxyalkyl, hydroxyalkenyl, alkylene (meth)acrylate, carbonyl, carboxyl, or sulfonato, or R and R′ taken together form a carbocyclic or hetero atom-containing ring, or R′ is a direct bond attaching to the phenyl ring; X is optional, but when present is halogen, alkyl, alkenyl, cycloalkyl, hydroxyalkyl, hydroxyalkenyl, alkoxy, amino, alkylene- or alkenylene-ether, alkylene(meth)acrylate, carbonyl, carboxyl, nitroso, sulfonate, hydroxyl or haloalkyl; and Y is —SO 2 NH—, —CONH—, —NH—, and —PO(NHCONHCSNH 2 )NH—; and n is 0 or 1 and m is 1 or 2, or

wherein R and R′ are independently selected from hydrogen, alkyl, alkenyl, aryl, hydroxyalkyl, hydroxyalkenyl, alkylene (meth)acrylate, carbonyl, carboxyl, or sulfonato, or R and R′ taken together form a carbocyclic or hetero atom-containing ring, or R′ is a direct bond attaching to the phenyl ring; X is optional, but when present is halogen, alkyl, alkenyl, cycloalkyl, hydroxyalkyl, hydroxyalkenyl, alkoxy, amino, alkylene- or alkenylene-ether, alkylene(meth)acrylate, carbonyl, carboxyl, nitroso, sulfonate, hydroxyl or haloalkyl; and Y is —SO 2 NH—, —CONH—, —NH—, and —PO(NHCONHCSNH 2 )NH—; and n is 0 or 1 and m is 1 or 2.

11. A composition comprising a bond formed between two mated substrates with the composition of claim 1 .

12. The composition of claim 1 , wherein the anaerobic cure accelerator is at least one of:

13. The composition of claim 1 , wherein the peroxide is selected from the group consisting of cumene hydroperoxide, para-menthane hydroperoxide, t-amyl hydroperoxide, 1,1,3,3-tetramethylbutyl hydroperoxide, t-butyl hydroperoxide, t-butyl perbenzoate, benzoyl peroxide, dibenzoyl peroxide, 1,3-bis(t-butylperoxyisopropyl)benzene, diacetyl peroxide, butyl 4,4-bis(t-butylperoxy)valerate, p-chlorobenzoyl peroxide, t-butyl cumyl peroxide, t-butyl perbenzoate, di-t-butyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di-t-butylperoxyhexane, 2,5-dimethyl-2,5-di-t-butyl-peroxyhex-3-yne, 4-methyl-2,2-di-t-butylperoxypentane, and combinations thereof.

Assignments (10)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 9, 2022
From: HENKEL IP & HOLDING GMBH
To: HENKEL AG & CO. KGAA
Reel/Frame 059357/0267 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 26, 2015
From: HENKEL US IP LLC
To: HENKEL IP & HOLDING GMBH
Reel/Frame 035100/0776 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 7, 2014
From: HENKEL CORPORATION
To: HENKEL US IP LLC
Reel/Frame 034184/0396 →
CORRECTIVE ASSIGNMENT TO CORRECT INCORRECT PROPERTIES 6620263, 8168743, 8642709, 8632654, 7973158, 12765973, 12766112, 13836858, 12945256, 13785007, 13785477, 13799002, 13840063 AND 13770295 PREVIOUSLY RECORDED ON REEL 032326 FRAME 0121. ASSIGNOR(S HEREBY CONFIRMS THE ASSIGNMENT. Recorded Sep 26, 2014
From: HENKEL AG & CO. KGAA
To: HENKEL IP & HOLDING GMBH
Reel/Frame 033860/0888 →
MERGER Recorded Feb 28, 2014
From: HENKEL IRELAND LIMITED
To: HENKEL AG & CO. KGAA
Reel/Frame 032373/0281 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 28, 2014
From: HENKEL AG & CO. KGAA
To: HENKEL IP & HOLDING GMBH
Reel/Frame 032326/0121 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 24, 2014
From: HENKEL AG & CO. KGAA
To: HENKEL IP & HOLDING GMBH
Reel/Frame 032329/0172 →
MERGER Recorded Feb 24, 2014
From: HENKEL IRELAND LIMITED
To: HENKEL AG & CO. KGAA
Reel/Frame 032329/0132 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 22, 2013
From: JACOBINE, ANTHONY F.; MESSANA, ANDREW D.; SCHALL, JOEL D.; HURLBURT, LYNNETTE
To: HENKEL CORPORATION
Reel/Frame 031454/0049 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 22, 2013
From: BIRKETT, DAVID P.; MULLEN, DAVID; WYER, MARTIN
To: HENKEL IRELAND LIMITED
Reel/Frame 031454/0215 →