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US3972863A
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Method for preparing copolymers from conjugated dienes and monovinylaromatic compounds with random distribution of monomer units
Assignee: Individual
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Filing: 1974-03-05
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Granted: 1976-08-03
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Expires: 1994-03-05
Abstract
Abstract A method of preparing copolymers of conjugated diene monomers and monovinylaromatic monomers having a random distribution of monomer units in the presence of a catalyst, metallic lithium in granules, and a modifying additive soluble in a reaction medium and consisting of reaction products of potassium or sodium carbonate, acetate or hydroxide with organoaluminum compound of the general formula: AlR' m R n , in which: R' -can be alkyl, aryl, aralkyl, group- OR'", -SR'" or -NR 2 '"; R" - is alkoxy or aryloxy radicals; R'"- -can be hydrogen, alkyl, aryl, aralkyl; m and n - are integers from 0 to 3, inclusive, in case of the said carbonates and acetates, m - are integers from 0 to 2, inclusive, and n-are integers from 1 to 3, inclusive, in case of the said hydroxides. In the above mentioned product the ratio of g-atoms of aluminum per 1 g-atom of potassium or sodium can be from 2 to 20. Copolymerization is effected in solution in liquid hydrogen solvent over a temperature range from 0° to 100°C.
Inventors
- 👤 Gennady Nikolaevich Petrov
- 👤 Gennady Mikhailovich Tolstopyatov
- 👤 Sergei Mikhailovich Krasilnikov
- 👤 Nikolai Alexandrovich Juzhakov
- 👤 Tatyana Alexeevna Kornilova
- 👤 Svetlana Mikhailovna Lashova
- 👤 Valentin Pavlovich Shatalov
- 👤 Leonid Vasillevich Kovtunenko
- 👤 Alexandr Julievich Shteinbok
- 👤 Elena Yakovlevna Mandelshtam
- 👤 Boris Sergeevich Korotkevich
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 16:25
CPC Classifications
C; C08; C08F; C08F236/00; C08F236/02; C08F236/04; C08F236/10
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
252 words
A method of preparing copolymers of conjugated diene monomers and monovinylaromatic monomers having a random distribution of monomer units which comprises copolymerizing said monomers in the presence of metallic lithium in granules as catalyst, and a modifying additive soluble in the reaction medium, said additive being the reaction product of a compound selected from the group consisting of potassium carbonate, potassium acetate, potassium hydroxide, sodium carbonate, sodium acetate and sodium hydroxide with an organoaluminum compound of the formula AlR m ' R n ", in which R' is selected from the group consisting of alkyl, aryl and aralkyl radicals, and radicals of the formula --OR"', --SR"', NR 2 "'; R" is selected from the group consisting of alkoxy and aryloxy radicals; R"' is selected from the group consisting of alkyl, aryl, aralkyl radicals and hydrogen; m and n are integers from 0 to 3, inclusive, for the reaction product of said organoaluminum compound with said carbonates and acetates; m are integers from 0 to 2, inclusive, and n are integers from 1 to 3, inclusive, for the reaction product of said organoaluminum compound with said hydroxides wherein the ratio of g-atoms of aluminum to 1 g-atom of sodium or potassium is from 2 to 20, said modifying additive being taken in an amount which corresponds to 1.10 - 5 to 2.10 - 1 g-atoms of aluminum per 100 g of said copolymerizing monomers; and said copolymerization being effected in solution in a liquid hydrocarbon solvent which is inert to the initial components.
Claim 2
Independent Claim
252 words
A method of preparing copolymers of conjugated diene monomers and monovinylaromatic monomers having a random distribution of monomer units which comprises copolymerizing said monomers in the presence of metallic lithium in granules as catalyst, and a modifying additive soluble in the reaction medium, said additive being the reaction product of a compound selected from the group consisting of potassium carbonate, potassium acetate, potassium hydroxide, sodium carbonate, sodium acetate and sodium hydroxide with an organoaluminum compound of the formula AlR m ' R n ", in which R' is selected from the group consisting of alkyl, aryl and aralkyl radicals, and radicals of the formula --OR"', --SR"', NR 2 "'; R" is selected from the group consisting of alkoxy and aryloxy radicals; R"' is selected from the group consisting of alkyl, aryl, aralkyl radicals and hydrogen; m and n are integers from 0 to 3, inclusive, for the reaction product of said organoaluminum compound with said carbonates and acetates; m are integers from 0 to 2, inclusive, and n are integers from 1 to 3, inclusive, for the reaction product of said organoaluminum compound with said hydroxides wherein the ratio of g-atoms of aluminum to 1 g-atom of sodium or potassium is from 2 to 20, said modifying additive being taken in an amount which corresponds to 1.10 - 5 to 2.10 - 1 g-atoms of aluminum per 100 g of said copolymerizing monomers; and said copolymerization being effected in solution in a liquid hydrocarbon solvent which is inert to the initial components.
Claim 3
Dependent Claim
35 words
A method as claimed in claim 1 wherein the modifying additive is used in an amount which corresponds to 1.10 - 4 to 1.10 - 3 g-atoms of aluminum per 100 g of copolymerizing monomers.
Claim 4
Dependent Claim
29 words
A method as claimed in claim 1 wherein the ratio of g-atoms of aluminum to g-atoms of potassium or sodium in the modifying additive is from 3 to 10.
Claim 5
Dependent Claim
30 words
A method as claimed in claim 2 wherein the ratio of g-atoms of aluminum to g-atoms of potassium or sodium in the modifying additive can be from 3 to 10.
Claim 6
Dependent Claim
32 words
A method as claimed in claim 1 wherein the modifying additive is the reaction product of isobutyldiisobutoxyaluminum with potassium hydroxide, the ratio of g-atoms of aluminum to g-atoms of potassium being 4.7.
Claim 7
Dependent Claim
32 words
A method as claimed in claim 2 wherein the modifying additive is the reaction product of isobutyldiisobutoxyaluminum with potassium hydroxide, the ratio of g-atoms of aluminum to g-atoms of potassium being 4.7.
Claim 8
Dependent Claim
17 words
A method as claimed in claim 1 wherein the copolymerization is effected at a temperature of 60°-80°C.
Claim 9
Dependent Claim
17 words
A method as claimed in claim 4 wherein the copolymerization is effected at a temperature of 60°-80°C.
Claim 10
Dependent Claim
17 words
A method as claimed in claim 6 wherein the copolymerization is effected at a temperature of 60°-80°C.
Claim 11
Dependent Claim
20 words
A method as claimed in claim 1 wherein the conjugated diene monomer is butadiene and the monovinylaromatic monomer is styrene.
Claim 12
Dependent Claim
20 words
A method as claimed in claim 7 wherein the conjugated diene monomer is butadiene and the monovinylaromatic monomer is styrene.
Claim 13
Dependent Claim
20 words
A method as claimed in claim 8 wherein the conjugated diene monomer is butadiene and the monovinylaromatic monomer is styrene.
Claim 14
Dependent Claim
20 words
A method as claimed in claim 9 wherein the conjugated diene monomer is butadiene and the monovinylaromatic monomer is styrene.
Claim 15
Dependent Claim
27 words
A method as claimed in claim 1 wherein the liquid hydrocarbon solvent is a mixture of hexane and toluene taken in a ratio from 0.5:1 to 10:1.
Claim 16
Dependent Claim
27 words
A method as claimed in claim 10 wherein the liquid hydrocarbon solvent is a mixture of hexane and toluene taken in a ratio from 0.5:1 to 10:1.
Claim 17
Dependent Claim
27 words
A method as claimed in claim 11 wherein the liquid hydrocarbon solvent is a mixture of hexane and toluene taken in a ratio from 0.5:1 to 10:1.
Claim 18
Dependent Claim
27 words
A method as claimed in claim 12 wherein the liquid hydrocarbon solvent is a mixture of hexane and toluene taken in a ratio from 0.5:1 to 10:1.
Claim 19
Dependent Claim
27 words
A method as claimed in claim 13 wherein the liquid hydrocarbon solvent is a mixture of hexane and toluene taken in a ratio from 0.5:1 to 10:1.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-08-03 | 1980-02-02 | 1980-08-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-08-03 | 1984-02-02 | 1984-08-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-08-03 | 1988-02-02 | 1988-08-03 | $7700.00 | Window Closed / Lapsed |