US4051308A
Expired / Lapsed
US
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Process for polymerizing butadiene with cobalt complex, AlR3 and CS2
Assignee: Bridgestone Firestone Inc
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Filing: 1975-11-06
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Granted: 1977-09-27
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Expires: 1995-11-06
Abstract
Abstract 1,3-Butadiene is polymerized in the liquid phase in the presence of a catalyst composition comprising: A. A complex of a cobalt salt; B. AlR 3 wherein R is hydrocarbon, and C. CS 2 . The complex comprises one of a cobalt salt, preferably CoCl 2 , with an organic compound containing nitrogen and oxygen or sulfur, preferably with no more than 2 carbon atoms separating the nitrogen and oxygen or sulfur, and the organometal reducing agent AlR 3 , wherein R is a hydrocarbon radical, preferably of no more than 10 carbon atoms. The polybutadiene has a microstructure of at least 80% and generally more than 90% 1,2, is also syndiotactic in character, has a melting point of 190°-227° C, and may be obtained in approximately quantitative yields.
Inventors
- 👤 Adel Farhan Halasa
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 21:45
CPC Classifications
C; C08; C08F; C08F136/00; C08F136/02; C08F136/04; C08F136/06
Claims Analysis
Total Claims: 15
Claim 1
Independent Claim
111 words
A process for the preparation of polybutadiene high in syndiotactic 1,2 structure range of 190°-227° C., which comprises polymerizing 1,3-butadiene in the liquid phase in the presence of a catalyst composition consisting essentially of: a. a complex of a cobalt salt selected from the class consisting of halides, carboxylates, carbonate and thiocarboxylates, said complex being formed with a cyclic compound having an amino nitrogen and a keto or thioketo group therein selected from the class consisting of N-methyl-pyrrolidone, pyrrolidone, caprolactam, p-aminoacetophenone, N,N-dimethyl-p-aminoacetophenone, N-methyl-2-aminocyclohexanone, N-methyl-thiopyrrolidone and thiocaprolactam; b. a reducing agent having the formula AIR 3 , wherein R is a hydrocarbon radical of 1-8 carbon atoms; and c. CS 2 .
Claim 2
Dependent Claim
111 words
A process for the preparation of polybutadiene high in syndiotactic 1,2 structure range of 190°-227° C., which comprises polymerizing 1,3-butadiene in the liquid phase in the presence of a catalyst composition consisting essentially of: a. a complex of a cobalt salt selected from the class consisting of halides, carboxylates, carbonate and thiocarboxylates, said complex being formed with a cyclic compound having an amino nitrogen and a keto or thioketo group therein selected from the class consisting of N-methyl-pyrrolidone, pyrrolidone, caprolactam, p-aminoacetophenone, N,N-dimethyl-p-aminoacetophenone, N-methyl-2-aminocyclohexanone, N-methyl-thiopyrrolidone and thiocaprolactam; b. a reducing agent having the formula AIR 3 , wherein R is a hydrocarbon radical of 1-8 carbon atoms; and c. CS 2 .
Claim 3
Dependent Claim
13 words
The process of claim 1 in which said reducing agent is triisobutyl aluminum.
Claim 4
Dependent Claim
14 words
The process of claim 1 in which said reducing agent is an aluminum trialkyl.
Claim 5
Dependent Claim
12 words
The process of claim 3 in which said complex former is N-methylpyrrolidone.
Claim 6
Dependent Claim
13 words
The process of claim 3 in which said complex former is a caprolactam.
Claim 7
Dependent Claim
12 words
The process of claim 3 in which said complex former is pyrrolidone.
Claim 8
Dependent Claim
13 words
The process of claim 3 in which said complex former is an p-amino-acetophenone.
Claim 9
Dependent Claim
26 words
The process of claim 7, in which said complex former is N-methylpyrrolidone and is used in a proportion of 1-16 moles per mole of Co salt.
Claim 10
Dependent Claim
13 words
The process of claim 8 in which said cobalt salt is cobaitous chloride.
Claim 11
Dependent Claim
26 words
The process of claim 9 in which said complex former is caprolactam and is used in a proportion of 1-6 moles per mole of Co salt.
Claim 12
Dependent Claim
13 words
The process of claim 10 in which said cobalt salt is cobaltous chloride.
Claim 13
Dependent Claim
65 words
The process of claim 1 in which 1-16 moles of complex former is used per mole of Co salt; said cobalt salt is used in a proportion of 0.02-0.1 millimoles per 100 grams of butadiene; the proportion of reducing agent is 25-75 moles of Al compound per mole of Co salt; and the proportion of CS 2 is 2-6 moles per mole of Co salt.
Claim 14
Dependent Claim
38 words
The process of claim 12 in which said reducing agent is a trialkyl aluminum, said complex former is N-methylpyrrolidone used in a proportion of 1-16 moles per mole of Co salt, and said cobalt salt is cobaltous chloride.
Claim 15
Dependent Claim
39 words
The process of claim 12 in which said reducing agent is a trialkyl aluminum, said complex former is caprolactam used in proportion of 1-6 moles of caprolactam per mole of Co salt, and said cobalt salt is cobaltous chloride.
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) | 1980-09-26 | 1981-03-28 | 1981-09-27 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-09-26 | 1985-03-28 | 1985-09-27 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-09-26 | 1989-03-28 | 1989-09-27 | $7700.00 | Window Closed / Lapsed |