IP Library Granted Patent US 7,473,815
Granted Patent B2
US 7,473,815 · App. 10/712,829 · Granted Jan 6, 2009

Process for removal of catalyst residues from poly-α-olefins

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Quick Facts
Patent No.
US 7,473,815
App. No.
10/712,829
Granted
Jan 6, 2009
Kind
B2
Abstract

A method is disclosed for reducing levels of residual halogen and Group IIIb metals in a crude poly(α-olefin) polymerized in the presence of a catalyst comprising the halogen and Group IIIb metals, wherein the method comprises: A) washing the crude poly(α-olefin) with water; B) separating the aqueous and organic phases; C) then adding an adsorbent selected from the group consisting of magnesium silicates, calcium silicates, aluminum silicates, aluminum oxides, and clays to the organic phase to form a slurry; D) heating the slurry under reduced pressure at a temperature of at least about 180° C. for at least about thirty minutes; and then E) separating the adsorbent from the slurry.

Claims (33)

1. A method of reducing levels of residual halogen to from 70 to 206 parts per million and reducing levels of residual Group IIIb metals to 0.1 or less parts per million in a liquid poly(α-olefin) polymerized in the presence of a catalyst comprising the halogen and Group IIIb metals, wherein the method comprises:

A) washing the liquid poly (α-olefin) with water;

B) separating the aqueous and organic phases;

C) then adding from 0.78-1.0 eq. metal/eq. halogen of an adsorbent selected from the group consisting of magnesium silicates, calcium silicates, aluminum silicates, aluminum oxides, and clays to the organic phase to form a slurry;

D) heating the slurry under a vacuum of at least 50 mmHg and at a temperature of at least about 180° C. for at least about thirty minutes; and then

E) separating the adsorbent from the slurry.

2. The method of claim 1 wherein the halogen is selected from the group consisting of chlorine, bromine, and mixtures thereof.

3. The method of claim 2 wherein the halogen is bromine.

4. The method of claim 1 wherein the Group IIIb metal is aluminum.

5. The method of claim 1 wherein the adsorbent is a magnesium silicate.

6. The method of claim 1 wherein the heating step is continued for at least about 90 minutes.

7. The method of claim 1 wherein the heating step is continued for at least about 180 minutes.

8. The method of claim 1 wherein the adsorbent is separated from the slurry by filtration.

9. A method of reducing levels of residual halogen to about 105 parts per million and reducing levels of residual Group IIIb metals to 0.1 or less parts per million in a liquid poly(α-olefin) polymerized in the presence of a catalyst comprising the halogen and Group IIIb metals, wherein the method comprises:

A) washing the liquid poly (α-olefin) with water;

B) separating the aqueous and organic phases;

C) then adding about 1.2 eq. metal/eq. halogen of an adsorbent selected from the group consisting of magnesium silicates, calcium silicates, aluminum silicates, aluminum oxides, and clays to the organic phase to form a slurry;

D) heating the slurry under a vacuum of at least 50 mmHg and at a temperature of at least about 180° C. for about 180 minutes; and then

E) separating the adsorbent from the slurry.

10. A method of reducing levels of residual halogen to from 70 to 206 parts per million and reducing levels of residual Group IIIb metals to 0.1 or less parts per million in a liquid poly(α-olefin) polymerized in the presence of a catalyst comprising the halogen and Group IIIb metals, wherein the method comprises:

A) washing the liquid poly (α-olefin) with water;

B) separating the aqueous and organic phases;

C) then adding from 0.78-1.0 eq. metal/eq. halogen of an adsorbent selected from the group consisting of magnesium silicates, calcium silicates, and aluminum silicates to the organic phase to form a slurry;

D) heating the slurry under a vacuum of at least 50 mmHg and at a temperature of at least about 180° C. for at least about thirty minutes; and then

E) separating the adsorbent from the slurry.

11. The method of claim 10 wherein the halogen is selected from the group consisting of chlorine, bromine, and mixtures thereof.

12. The method of claim 11 wherein the halogen is bromine.

13. The method of claim 10 wherein the Group IIIb metal is aluminum.

14. The method of claim 10 wherein the adsorbent is a magnesium silicate.

15. The method of claim 10 wherein the heating step is continued for at least about 90 minutes.

16. The method of claim 10 wherein the heating step is continued for at least about 180 minutes.

17. The method of claim 10 wherein the adsorbent is separated from the slurry by filtration.

18. The method of claim 13 wherein the adsorbent is a magnesium silicate.

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 Feb 12, 2004
From: LAMBERT TIMOTHY; THURING, WERNER
To: CROMPTON CORPORATION
Reel/Frame 014975/0173 →