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Patent US4360643A successfully refreshed from Google Patents.
US4360643A
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Method of preparing lactone block copolymers
Assignee: Phillips Petroleum Co
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Filing: 1980-07-16
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Granted: 1982-11-23
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Expires: 2000-07-16
Abstract
Abstract A method is provided for producing block copolymers of a lactone and a conjugated diene and/or a monovinylarene, in which the lactone polymerization step is terminated by addition of water, a mineral acid or a carboxylic acid.
Inventors
- 👤 Floyd E. Naylor
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 18:57
CPC Classifications
C; C08; C08G; C08G63/00; C08L; C08L67/00; C08L67/06
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
158 words
A method of preparing a lactone copolymer which comprises the steps of: (a) providing a lithium-terminated polymer of the form A--D--Li) y wherein A is a polymer segment comprising one or more polymer blocks of one or more conjugated dienes and/or monovinylarenes, D is a polymer segment comprising one or more polymer blocks of one or more lactones, and y is 1, 2, 3 or 4, the lithium-terminated polymer being present in a diluent selected from the group consisting of paraffins, cycloparaffins and aromatic hydrocarbons; (b) contacting the lithium-terminated polymer with water to form (1) a lactone copolymer of the form A--D) y which is present in an organic phase comprising the lactone copolymer A--D) y and the diluent and (2) a water-soluble lithium hydroxide termination product which is present in a separate phase from the organic phase, the separate phase comprising water and lithium hydroxide; and (c) recovering the lactone copolymer of the form A--D) y .
Claim 2
Independent Claim
158 words
A method of preparing a lactone copolymer which comprises the steps of: (a) providing a lithium-terminated polymer of the form A--D--Li) y wherein A is a polymer segment comprising one or more polymer blocks of one or more conjugated dienes and/or monovinylarenes, D is a polymer segment comprising one or more polymer blocks of one or more lactones, and y is 1, 2, 3 or 4, the lithium-terminated polymer being present in a diluent selected from the group consisting of paraffins, cycloparaffins and aromatic hydrocarbons; (b) contacting the lithium-terminated polymer with water to form (1) a lactone copolymer of the form A--D) y which is present in an organic phase comprising the lactone copolymer A--D) y and the diluent and (2) a water-soluble lithium hydroxide termination product which is present in a separate phase from the organic phase, the separate phase comprising water and lithium hydroxide; and (c) recovering the lactone copolymer of the form A--D) y .
Claim 3
Dependent Claim
148 words
The method of claim 1 wherein the conjugated dienes are selected from the group consisting of conjugated diene monomers having 4 to 12, inclusive, carbon atoms per molecule, the monovinylarenes are selected from the group consisting of monovinylarene monomers having 8 to 12, inclusive, carbon atoms per molecule, and the lactones are selected from the group of lactone monomers represented by the formula ##STR3## wherein each R is selected independently from the group consisting of hydrogen, alkyl, cycloalkyl, aryl, alkenyl, cycloalkenyl, alkaryl and aralkyl; R' is selected from the group consisting of R, hydrogen and a radical of the formula ##STR4## and, when R' is the radical ##STR5## no R is attached to the carbon atom to which the radical is attached; the total number of carbon atoms in all the R and R' substituents does not exceed 12; and x is selected from 1, 3 and 4.
Claim 4
Dependent Claim
10 words
The method of claim 2 wherein the lactone is epsilon-caprolactone.
Claim 5
Dependent Claim
16 words
The method of claim 2 wherein the cojugated diene is 1,3-butadiene and the monovinylarene is styrene.
Claim 6
Dependent Claim
43 words
The method of claim 2 wherein the lithium-terminated polymer A--D--Li) y is formed by contacting a base polymer of the form A--Li) y with one or more lactone monomers in amounts sufficient and under conditions suitable to cause polymerization of the lactone monomers.
Claim 7
Dependent Claim
66 words
The method of claim 5 wherein the base polymer of the form A--Li) y is formed by reacting an organolithium initiator of the form R"(Li) y , wherein R" is a hydrocarbon radical selected from the group consisting of aliphatic, cycloaliphatic and aromatic radicals, with one or more monomers of A in amounts sufficient and under conditions suitable to cause polymerization of the monomers of A.
Claim 8
Dependent Claim
25 words
The method of claim 2 wherein A further comprises a residue of a capping agent selected from the group consisting of oxiranes, aldehydes and ketones.
Claim 9
Dependent Claim
12 words
The method of claim 7 wherein the capping agent is propylene oxide.
Claim 10
Dependent Claim
32 words
The method of claim 7 in which the conjugated diene is 1,3-butadiene, the monovinylarene is styrene, the lactone is epsilon-caprolactone, the organolithium initiator is b-butyllithium, and the capping agent is propylene oxide.
Claim 11
Dependent Claim
39 words
The method of claim 2, 4, 6, 8 or 9 in which the lithium-terminated polymer of the form A--D--Li) y is contacted with water at or before substantially quantitative conversion of the one or more lactone monomers to polymer.
Claim 12
Dependent Claim
11 words
The method of claim 10 in which the diluent is cyclohexane.
Claim 13
Dependent Claim
41 words
The method of claim 10 in which the polymer of the form A--D) y contains no more than a minor amount of units of the form A n Z(H) n , in which Z is the residue of a coupling agent.
Claim 14
Dependent Claim
27 words
The method of claim 10 wherein the thus terminated lactone copolymer contains a polymer segment D which cnstitutes at least 24 weight percent of A plus D.
Claim 15
Dependent Claim
30 words
The method of claim 10 wherein the thus terminated lactone copolymer contains a polymer segment D which constitutes from about 24 to about 40 weight percent of A plus D.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-11-22 | 1986-05-24 | 1986-11-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-11-22 | 1990-05-24 | 1990-11-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-11-22 | 1994-05-24 | 1994-11-23 | $7700.00 | Window Closed / Lapsed |