US3911054A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for lowering the viscosity of a solution of a living polymer
Assignee: Stamicarbon BV
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Filing: 1972-09-28
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Granted: 1975-10-07
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Expires: 1992-09-28
Abstract
Abstract Polyfunctional Lewis bases such as N,N,N'',N''-tetramethyl-1,2diaminoethane are used to lower the viscosity of a solution of a living polymer, especially during the preparation of a living polymer using a polyfunctional anionic initiator according to the process disclosed. Homopolymers and copolymers may be produced; the process is particularly suited for the preparation of A-B-A block copolymers the Lewis base being added after at least 50 percent of the first-formed polymer block is completed.
Inventors
- 👤 Bernard C Roest
- 👤 Emanuel M J Pijpers
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 15:33
CPC Classifications
C; C08; C08F; C08F297/00; C08F297/02; C08F297/04; C08F297/042; C08F36/00; C08F36/02; C08F36/04; C08F4/00; C08F4/06; C08F4/12
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
150 words
A PROCESS FOR LOWERING THE VISCOSITY OF A SOLUTION OF A LIVING POLYMER PRODUCED BY POLYMERIZING AT LEAST ONE CONJGATED DIENE MONOMER OF 4-18 CARBON ATOMS AND THEN COPOLMERIZING SAID DIENE WITH AN ANINOICALLY POLYMERIZABLE MONOMER SELECTED FROM THE ROUP CONSISTING OF METHYL METHACRYLATE, ACRYLONTRILE, STRENE, A-METHYLSTYRENE AND MIXTURES THEREOF, WHICH COMPRISES REACTING AT LEAST ONE CONJUGATED DIENE MONOMER AT A TEMPERATURE OF ABOUT +40* TO +80*C IN AN ORGANIC SOLVENT IN THE PRESENCE OF 0.05 TO 10 MMOLE OF A TITHIUM-CONTAINING POLYFUNCTIONAL ANIONIC INITATOR PER LITER OF THE SOLVENT FOR SAID DIENE MONOMER, AND THEREAFTER, AFTER AT LEAST 50 WEIGHT PERCENT OF SAID DIENE MONOMER HAS BEEN POLYMERIZED, CONSISTING OF ADDING IN THE LATEST STAGE OF THE POLYMERIZATION PROCESS THE LEWIS BASE N,N,N,N'',N''-TETRAMETHYL-1, 2-DISAMINOETHANE(TMEDA) IN THE AMOUNT OF FROM ABOUT 0.01 TO ABOUT 1000 TIMES OF SAID POLYFUNCTIONAAL ANIONIC INITIATOR THEREBY FORMING A CHELATE WITH LITHIUM POLYFUNCTIONAL ANIONIC INITATOR.
Claim 2
Dependent Claim
150 words
A PROCESS FOR LOWERING THE VISCOSITY OF A SOLUTION OF A LIVING POLYMER PRODUCED BY POLYMERIZING AT LEAST ONE CONJGATED DIENE MONOMER OF 4-18 CARBON ATOMS AND THEN COPOLMERIZING SAID DIENE WITH AN ANINOICALLY POLYMERIZABLE MONOMER SELECTED FROM THE ROUP CONSISTING OF METHYL METHACRYLATE, ACRYLONTRILE, STRENE, A-METHYLSTYRENE AND MIXTURES THEREOF, WHICH COMPRISES REACTING AT LEAST ONE CONJUGATED DIENE MONOMER AT A TEMPERATURE OF ABOUT +40* TO +80*C IN AN ORGANIC SOLVENT IN THE PRESENCE OF 0.05 TO 10 MMOLE OF A TITHIUM-CONTAINING POLYFUNCTIONAL ANIONIC INITATOR PER LITER OF THE SOLVENT FOR SAID DIENE MONOMER, AND THEREAFTER, AFTER AT LEAST 50 WEIGHT PERCENT OF SAID DIENE MONOMER HAS BEEN POLYMERIZED, CONSISTING OF ADDING IN THE LATEST STAGE OF THE POLYMERIZATION PROCESS THE LEWIS BASE N,N,N,N'',N''-TETRAMETHYL-1, 2-DISAMINOETHANE(TMEDA) IN THE AMOUNT OF FROM ABOUT 0.01 TO ABOUT 1000 TIMES OF SAID POLYFUNCTIONAAL ANIONIC INITIATOR THEREBY FORMING A CHELATE WITH LITHIUM POLYFUNCTIONAL ANIONIC INITATOR.
Claim 3
Dependent Claim
27 words
The process according to claim 1 wherein the Lewis base is used in an amount from about 0.1-10 times the molar quantity of the anionic polymerization initiator.
Claim 4
Dependent Claim
172 words
adding at least one monomer to the reaction mixture containing said block B and continuing said polymerization and under such conditions to form polymer blocks A on said polymer block B, polymer blocks A selected from the group consisting of a non-elastomeric homopolymer having a glass transition temperature over 25*C and a number average molecular weight between 2,000 and 50,000 and a non-elastomeric copolymer having a glass transition temperature over 25*C and a number average molecular weight between 2,000 and 50,000 whereby said block copolymer A-B-A is formed. the improvement consisting of adding the Lewis base N,N,N'',N''-tetramethyl-1-2 diaminoethane (TMEDA) to the polymerization mixture of step (1) after at least about 50 weight percent of said polymer block B has been formed and before at least 10 weight percent of polymer blocks A are formed said TMEDA present in the amount of from about 0.01 to 100 times the amount of said polylithium anionic initiator, said Lewis base capable of forming a chelate with the lithium ion of the polylithium anionic polymerization initiator.
Claim 5
Dependent Claim
172 words
adding at least one monomer to the reaction mixture containing said block B and continuing said polymerization and under such conditions to form polymer blocks A on said polymer block B, polymer blocks A selected from the group consisting of a non-elastomeric homopolymer having a glass transition temperature over 25*C and a number average molecular weight between 2,000 and 50,000 and a non-elastomeric copolymer having a glass transition temperature over 25*C and a number average molecular weight between 2,000 and 50,000 whereby said block copolymer A-B-A is formed. the improvement consisting of adding the Lewis base N,N,N'',N''-tetramethyl-1-2 diaminoethane (TMEDA) to the polymerization mixture of step (1) after at least about 50 weight percent of said polymer block B has been formed and before at least 10 weight percent of polymer blocks A are formed said TMEDA present in the amount of from about 0.01 to 100 times the amount of said polylithium anionic initiator, said Lewis base capable of forming a chelate with the lithium ion of the polylithium anionic polymerization initiator.
Claim 6
Dependent Claim
131 words
adding styrene monomer to the reaction mixture containing said block B and continuing said polymerization and under such conditions to form polymer blocks A on said polymer block B, polymer blocks A having a number average molecular weight between 2,000 and 50,000 whereby said block copolymer A-B-A is formed, the improvement consisting of adding to the Lewis base N,N,N'', N''-tetramethyl-1,2 diaminoethane (TMEDA) to the polymerization mixture of step (1) after at least about 50 weight percent of said polymer block B has been formed and before at least 10 weight percent of polymer blocks A are formed, said TMEDA present in the amount of from about 0.01 to 100 times the amount of said polylithium anionic initiator, thereby forming a chelate with the lithium ion of the polylithium anionic polymerization initiator.
Claim 7
Dependent Claim
131 words
adding styrene monomer to the reaction mixture containing said block B and continuing said polymerization and under such conditions to form polymer blocks A on said polymer block B, polymer blocks A having a number average molecular weight between 2,000 and 50,000 whereby said block copolymer A-B-A is formed, the improvement consisting of adding to the Lewis base N,N,N'', N''-tetramethyl-1,2 diaminoethane (TMEDA) to the polymerization mixture of step (1) after at least about 50 weight percent of said polymer block B has been formed and before at least 10 weight percent of polymer blocks A are formed, said TMEDA present in the amount of from about 0.01 to 100 times the amount of said polylithium anionic initiator, thereby forming a chelate with the lithium ion of the polylithium anionic polymerization initiator.
Claim 8
Dependent Claim
32 words
The process according to claim 1 wherein the Lewis base is added in the latest stage of the polymerization process after at least about 75 weight percent of said monomer is polymerized.
Claim 9
Dependent Claim
36 words
In a process for the preparation of a block copolymer having good physical and mechanical properties of the general configuration A-B-A in the presence of a polylithium anionic polymerization initiator comprising the sequential polymerization steps of:
Claim 10
Dependent Claim
36 words
In a process for the preparation of a block copolymer having good physical and mechanical properties of the general configuration A-B-A in the presence of a polylithium anionic polymerization initiator comprising the sequential polymerization steps of:
Claim 11
Dependent Claim
27 words
The process according to claim 4 wherein the Lewis base is used in an amount from about 0.01-10 times the molar quantity of the anionic polymerization initiator.
Claim 12
Dependent Claim
36 words
In a process for the preparation of a block copolymer having improved physical and mechanical properties of the general configuration A-B-A in the presence of a polylithium anionic polymerization initiator comprising the sequential polymerization steps of:
Claim 13
Dependent Claim
36 words
In a process for the preparation of a block copolymer having improved physical and mechanical properties of the general configuration A-B-A in the presence of a polylithium anionic polymerization initiator comprising the sequential polymerization steps of:
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) | 1978-10-06 | 1979-04-07 | 1979-10-07 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-10-06 | 1983-04-07 | 1983-10-07 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-10-06 | 1987-04-07 | 1987-10-07 | $7700.00 | Window Closed / Lapsed |