IP Library Granted Patent US 7,189,875
Granted Patent B2
US 7,189,875 · App. 10/815,578 · Granted Mar 13, 2007

Diphenylamine alkylated with olefin mixtures containing fractions with varying degrees of activity

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Quick Facts
Patent No.
US 7,189,875
App. No.
10/815,578
Granted
Mar 13, 2007
Kind
B2
Abstract

Disclosed herein is a process for the preparation of alkylated diarylamines comprising adding to said diarylamine an olefin mixture containing highly reactive fractions, as well as fractions exhibiting a relatively lower chemical reactivity, in the presence of an acidic clay catalyst at a temperature low enough to prevent substantial deactivation of the catalyst until the addition is complete and then increasing the temperature to increase the alkylation rate of the less reactive fractions.

Claims (13)

1. An alkylated diphenylamine of the general formula:

wherein R 1 , R 2 , R 3 , and R 4 are independently selected from the group consisting of hydrogen, oligomers of isobutylene, and oligomers of propylene, provided that at least one of R 1 , R 2 , R 3 , and R 4 is not hydrogen, prepared by a process comprising adding to a diphenylamine a mixture of oligomers of isobutylene or a mixture of oligomers of propylene in which said mixtures comprise highly reactive fractions, as well as fractions having lesser reactivity, in the presence of an acidic clay catalyst at a temperature low enough to prevent substantial deactivation of the catalyst until the addition is complete and then increasing the temperature to increase the alkylation rate of the less reactive fractions to yield a product that comprises 0.1 to 1% diphenylamine, <10% tert-butyl diphenylamine, <10% di-tert-butyl diphenylamine, <10% mono-octyl diphenylamine, >20% dodecyl diphenylamine, >15% hexadecyl diphenylamine, <10% eicosenyl diphenylamine, <7% tetracosenyl diphenylamine, <4% octacosenyl diphenylamine and <2% polyisobutyl diphenylamine.

2. The alkylated diphenylamine of claim 1 wherein no more that 27% of the total reaction mixture is comprised of C 8 alkylation or less, and no more than 15% of the total reaction mixture is comprised of C 24 alkylation or more.

3. The alkylated diphenylamine of claim 1 wherein the isobutylene oligomer has a number average molecular weight of about 120 to about 600 and a methylvinylidene content of at least about 25%.

4. A composition comprising:

A) an organic product selected from the group consisting of lubricants, hydraulic fluids, metal-working fluids, fuels, and polymers; and

B) a stabilizing amount of an alkylated diphenylamine of the general formula:

wherein R 1 , R 2 , R 3 , and R 4 are independently selected from the group consisting of hydrogen, oligomers of isobutylene, and oligomers of propylene, provided that at least one of R 1 , R 2 , R 3 , and R 4 is not hydrogen, prepared by a process comprising adding to a diphenylamine a mixture of oligomers of isobutylene or a mixture of oligomers of propylene in which said mixtures comprise highly reactive fractions, as well as fractions having lesser reactivity, in the presence of an acidic clay catalyst at a temperature low enough to prevent substantial deactivation of the catalyst until the addition is complete and then increasing the temperature to increase the alkylation rate of the less reactive fractions to yield a product that comprises 0.1 to 1% diphenylamine, <10% tert-butyl diphenylamine, <10% di-tert-butyl diphenylamine, <10% mono-octyl diphenylamine, >20% dodecyl diphenylamine, >15% hexadecyl diphenylamine, <10% eicosenyl diphenylamine, <7% tetracosenyl diphenylamine, <4% octacosenyl diphenylamine and <2% polyisobutyl diphenylamine.

5. The composition of claim 4 wherein no more that 27% of the total reaction mixture of the alkylated diphenylamine is comprised of C 8 alkylation or less, and no more than 15% of the total reaction mixture is comprised of C 24 alkylation or more.

6. The composition of claim 4 wherein the isobutylene oligomer that is added to the diphenylamine has a number average molecular weight of about 120 to about 600 and a methylvinylidene content of at least about 25%.

7. The composition of claim 4 wherein the alkylated diphenylamine is present in concentrations of from about 0.05 to about 10.0% by weight based on the material to be stabilized.

8. The composition of claim 4 wherein the organic product is a lubricating oil.

9. The composition of claim 4 wherein the organic product is an elastomer.

Assignments (11)
CHANGE OF NAME Recorded Sep 25, 2018
From: CROMPTON CORPORATION
To: CHEMTURA CORPORATION
Reel/Frame 047141/0152 →
RELEASE OF FIRST LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded May 11, 2017
From: BANK OF AMERICA, N.A.
To: CHEMTURA CORPORATION; BIOLAB FRANCHISE COMPANY, LLC; BIO-LAB, INC.; CROMPTON COLORS INCORPORATED; CROMPTON HOLDING CORPORATION; GLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; LAUREL INDUSTRIES HOLDINGS, INC.; RECREATIONAL WATER PRODUCTS, INC.; WEBER CITY ROAD LLC
Reel/Frame 042447/0508 →
RELEASE OF SECOND LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded May 11, 2017
From: BANK OF AMERICA, N.A.
To: CHEMTURA CORPORATION; BIOLAB FRANCHISE COMPANY, LLC; BIO-LAB, INC.; CROMPTON COLORS INCORPORATED; CROMPTON HOLDING CORPORATION; GLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; LAUREL INDUSTRIES HOLDINGS, INC.; RECREATIONAL WATER PRODUCTS, INC.; WEBER CITY ROAD LLC
Reel/Frame 042449/0001 →
SECDOND LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded Mar 21, 2011
From: CHEMTURA CORPORATION; BIOLAB FRANCHISE COMPANY, LLC; BIO-LAB, INC.; CROMPTON COLORS INCORORATED; CROMPTON HOLDING CORPORATION; CLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; HAOMECARE LABS, INC.; LAUREL INDUSTRIES HOLDINGS, INC.; RECREATIONAL WATER PRODUCTS, INC.; WEBER CITY ROAD LLC
To: BANK OF AMERICA, N. A.
Reel/Frame 027881/0347 →
FIRST LIEN INTELLECTUAL PROPERTY SECURITY AGREEMENT. Recorded Mar 21, 2011
From: CHEMTURA CORPORATION; BIOLAB FRANCHISE COMPANY, LLC; BIO-LAB, INC.; CROMPTON COLORS INCORPORATED; CROMPTON HOLDING CORPORATION; GLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; LAUREL INDUSTRIES HOLDINGS, INC.; RECREATIONAL WATER PRODUCTS, INC.; WEBER CITY ROAD LLC
To: BANK OF AMERICA, N.A.
Reel/Frame 026028/0622 →
INTELLECTUAL PROPERTY SECURITY RELEASE AGREEMENT Recorded Mar 21, 2011
From: CITIBANK, N.A.
To: CHEMTURA CORPORATION; A & M CLEANING PRODUCTS, LLC; ASCK, INC; BIOLAB COMPANY STORE, LLC; AQUA CLEAR INDUSTRIES, LLC; ASEPSIS, INC.; BIOLAB TEXTILES ADDITIVES, LLC; BIOLAB, INC.; CROMPTON COLORS INCORPORATED; CROMPTON MONOCHEM, INC.; CNK CHEMICAL REALTY CORPORATION; CROMPTON HOLDING CORPORATION; GLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GT SEED TREATMENT, INC.; ISCI, INC; GREAT LAKES CHEMICAL GLOBAL, INC.; HOMECARE LABS, INC.; KEM MANUFACTURING CORPORATION; LAUREL INDUSTRIES HOLDINGS, INC.; NAUGATUCK TREATMENT COMPANY; UNIROYAL CHEMICAL COMPANY LIMITED (DELAWARE); MONOCHEM, INC.; RECREATIONAL WATER PRODUCTS, INC.; WEBER CITY ROAD LLC; WRL OF INDIANA, INC.; BIOLAB FRANCHISE COMPANY, LLC
Reel/Frame 026039/0142 →
AMENDED AND RESTATED INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded Feb 22, 2010
From: CHEMTURA CORPORATION; A & M CLEANING PRODUCTS, LLC; AQUA CLEAR INDUSTRIES, LLC; ASCK, INC.; ASEPSIS, INC.; BIOLAB COMPANY STORE, LLC; BIOLAB FRANCHISE COMPANY, LLC; BIOLAB TEXTILE ADDITIVES, LLC; BIO-LAB, INC.; CNK CHEMICAL REALTY CORPORATION; CROMPTON COLORS INCORPORATED; CROMPTON HOLDING CORPORATION; CROMPTON MONOCHEM, INC.; GLCC LAUREL, LLC; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; ISCI, INC.; KEM MANUFACTURING CORPORATION; LAUREL INDUSTRIES HOLDINGS, INC.; MONOCHEM, INC.; NAUGATUCK TREATMENT COMPANY; RECREATIONAL WATER PRODUCTS, INC.; UNIROYAL CHEMICAL COMPANY LIMITED (DELAWARE); WEBER CITY ROAD LLC; WRL OF INDIANA, INC.
To: CITIBANK, N.A.
Reel/Frame 023998/0001 →
SECURITY AGREEMENT Recorded May 12, 2009
From: CHEMTURA CORPORATION; A & M CLEANING PRODUCTS, LLC; AQUA CLEAR INDUSTRIES, LLC; ASCK, INC.; ASEPSIS, INC.; BIOLAB TEXTILE ADDITIVES, LLC; BIO-LAB, INC.; CNK CHEMICAL REALTY CORPORATION; CROMPTON HOLDING CORPORATION; CROMPTON COLORS INCORPORATED; CROMPTON MONOCHEM, INC.; GREAT LAKES CHEMICAL CORPORATION; GREAT LAKES CHEMICAL GLOBAL, INC.; GT SEED TREATMENT, INC.; HOMECARE LABS, INC.; ISCI, INC.; KEM MANUFACTURING CORPORATION; LAUREL INDUSTRIES HOLDINGS, INC.; MONOCHEM, INC.; NAUGATUCK TREATMENT COMPANY; RECREATIONAL WATER PRODUCTS, INC.; UNIROYAL CHEMICAL COMPANY LIMITED (DELAWARE); WEBER CITY ROAD LLC; WRL OF INDIANA, INC.; BIOLAB COMPANY STORE, LLC; BIOLAB FRANCHISE COMPANY, LLC; GLCC LAUREL, LLC
To: CITIBANK, N.A.
Reel/Frame 022668/0658 →
RELEASE OF LIEN IN PATENTS Recorded Jul 13, 2005
From: DEUTSCHE BANK AG, NEW YORK BRANCH
To: CROMPTON CORPORATION
Reel/Frame 016513/0745 →
SECURITY AGREEMENT Recorded Nov 10, 2004
From: CROMPTON CORPORATION
To: DEUTSCHE BANK AG NEW YORK BRANCH
Reel/Frame 015370/0467 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 29, 2004
From: DUYCK, KARL J; LAMBERT, TIMOTHY L
To: CROMPTON CORPORATION
Reel/Frame 014790/0720 →