US4049732A
Expired / Lapsed
US
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Continuous telomerization process and its liquid products
Assignee: Lithium Corp of America Inc
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Filing: 1976-09-22
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Granted: 1977-09-20
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Expires: 1996-09-22
Abstract
Abstract Continuous process and apparatus for the preparation of normally liquid telomers derived from the reaction of a liquid telogen, such as toluene, with a polymerizable monomeric taxogen in gaseous form, such as 1,3-butadiene monomer, in the presence of an organometal telomerization initiator, such as a mixture or complex of n-butyllithium and potassium t-butoxide, wherein a controlled stream of the gaseous taxogen is continuously passed through fine apertures, as in a screen, into the liquid telogen containing said initiator disposed in a reaction zone in a reaction chamber, whereby to produce the normally liquid telomer, and, thereafter said telomer is continuously passed through a conduit into an additional reaction zone or zones and reacted in similar manner with additional gaseous taxogen until the desired concentration of liquid telomer is produced. The process is most desirably carried out in a controlled manner to prevent any undesirable excess of the taxogen from accumulating during the chain transfer step of the telomerization process. The process also results in the production of novel liquid telomers or liquid telomers having novel and advantageous properties in relation to otherwise generally similar liquid telomers heretofore known to the art.
Inventors
- 👤 Ricardo O. Bach
- 👤 Robert C. Morrison
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 05:28
CPC Classifications
C; C08; C08F; C08F2/00; C08F2/38; Y; Y10; Y10S; Y10S585/00; Y10S585/919; Y10S585/921; Y10S585/922; Y10S585/924; Y10S585/926; Y10S585/929; Y10S585/93; Y10S585/931
Claims Analysis
Total Claims: 29
Claim 1
Independent Claim
134 words
In a continuous process of producing normally liquid telomers wherein a liquid telogen is metalated with an organometal initiator and said metalated telogen is then reacted with at least one gaseous taxogen selected from the group of conjugated dienes and vinyl-substituted aromatic compounds, the steps which comprise forming a solution of said initiator and said telogen, continuously passing said solution to a first reaction zone, continuously passing a controlled stream of said gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution to effect telomerization of the telogen in said first reaction zone, continuously passing the resulting intermixture containing liquid telomer into a second reaction zone while continuously passing said gaseous taxogen through fine apertures into said intermixture containing liquid telomer to produce additional quantities of telomer.
Claim 2
Dependent Claim
134 words
In a continuous process of producing normally liquid telomers wherein a liquid telogen is metalated with an organometal initiator and said metalated telogen is then reacted with at least one gaseous taxogen selected from the group of conjugated dienes and vinyl-substituted aromatic compounds, the steps which comprise forming a solution of said initiator and said telogen, continuously passing said solution to a first reaction zone, continuously passing a controlled stream of said gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution to effect telomerization of the telogen in said first reaction zone, continuously passing the resulting intermixture containing liquid telomer into a second reaction zone while continuously passing said gaseous taxogen through fine apertures into said intermixture containing liquid telomer to produce additional quantities of telomer.
Claim 3
Dependent Claim
205 words
In a continuous process of producing normally liquid telomers wherein a liquid telogen is metalated with an organometal initiator and said metalated telogen is then reacted with at least one gaseous taxogen selected from the group of conjugated dienes and vinyl-substituted aromatic compounds, the steps which comprise forming a solution of said initiator and said telogen whereby to metalate the telogen, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of said gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution in said reaction zone to effect telomerization of the telogen in said first reaction zone, continuously passing the resulting intermixture containing liquid telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing said gaseous taxogen through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer, polymerization of said taxogen occurring as the stream continues its passage through said first reactor, followed by remetalation as said stream continues its passage through said first reactor and prior to its passage into said second reactor.
Claim 4
Dependent Claim
205 words
In a continuous process of producing normally liquid telomers wherein a liquid telogen is metalated with an organometal initiator and said metalated telogen is then reacted with at least one gaseous taxogen selected from the group of conjugated dienes and vinyl-substituted aromatic compounds, the steps which comprise forming a solution of said initiator and said telogen whereby to metalate the telogen, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of said gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution in said reaction zone to effect telomerization of the telogen in said first reaction zone, continuously passing the resulting intermixture containing liquid telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing said gaseous taxogen through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer, polymerization of said taxogen occurring as the stream continues its passage through said first reactor, followed by remetalation as said stream continues its passage through said first reactor and prior to its passage into said second reactor.
Claim 5
Dependent Claim
16 words
The process of claim 2, in which the telogen is toluene and the taxogen is 1,3-butadiene.
Claim 6
Dependent Claim
12 words
The process of claim 3, in which the initiator is an organolithium.
Claim 7
Dependent Claim
18 words
The process of claim 4, in which the organolithium initiator comprises a complex of n-butyllithium and potassium t-butoxide.
Claim 8
Dependent Claim
17 words
The process of claim 4, in which the organolithium initiator comprises a complex of n-butyllithium and N,N,N',N'-tetramethylethylenediamine.
Claim 9
Dependent Claim
17 words
The process of claim 4, in which the organolithium initiator comprises a complex of dilithiodiisoprene and N,N,N',N'-tetramethylethylenediamine.
Claim 10
Dependent Claim
18 words
The process of claim 3, in which the organolithium initiator is a complex of n-butyllithium and potassium t-butoxide.
Claim 11
Dependent Claim
17 words
The process of claim 3, in which the organolithium initiator is a complex of n-butyllithium and N,N,N',N'-tetramethylethylenediamine.
Claim 12
Dependent Claim
17 words
The process of claim 3, in which the organolithium initiator comprises a complex of dilithiodiisoprene and N,N,N',N'-tetramethylethylenediamine.
Claim 13
Dependent Claim
155 words
In a continuous process of producing normally liquid telomers wherein toluene is metalated with an organometal initiator and said metalated toluene is then reacted with gaseous 1,3-butadiene, said initiator comprising a complex of n-butyllithium and potassium t-butoxide, the steps which comprise forming a solution of said initiator and said toluene, with or without an inert organic solvent, whereby to metalate the toluene, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of gaseous 1,3-butadiene through fine apertures into said first reaction zone into direct contact with said initiator solution in said reaction zone, continuously passing the resulting intermixture containing telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing gaseous 1,3-butadiene through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer.
Claim 14
Dependent Claim
155 words
In a continuous process of producing normally liquid telomers wherein toluene is metalated with an organometal initiator and said metalated toluene is then reacted with gaseous 1,3-butadiene, said initiator comprising a complex of n-butyllithium and potassium t-butoxide, the steps which comprise forming a solution of said initiator and said toluene, with or without an inert organic solvent, whereby to metalate the toluene, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of gaseous 1,3-butadiene through fine apertures into said first reaction zone into direct contact with said initiator solution in said reaction zone, continuously passing the resulting intermixture containing telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing gaseous 1,3-butadiene through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer.
Claim 15
Dependent Claim
26 words
The process of claim 1, wherein said fine apertures having a size corresponding to a diameter in the range of about 2 to about 40 microns.
Claim 16
Dependent Claim
26 words
The process of claim 2, wherein said fine apertures having a size corresponding to a diameter in the range of about 2 to about 40 microns.
Claim 17
Dependent Claim
26 words
The process of claim 8, wherein said fine apertures having a size corresponding to a diameter in the range of about 2 to about 40 microns.
Claim 18
Dependent Claim
23 words
The process of claim 2, in which the rate of admission of the taxogen is maintained essentially constant to each of said reactors.
Claim 19
Dependent Claim
27 words
The process of claim 2, in which the initiator to taxogen ratio is controlled to maintain it essentially constant throughout the process of forming said liquid telomers.
Claim 20
Dependent Claim
30 words
The process of claim 8, in which the process is controlled whereby substantially the same number of polybutadiene molecules of equivalent molecular weight is formed in each of the reactors.
Claim 21
Dependent Claim
179 words
In a continuous process of producing normally liquid telomers in which there are interacted, as essential ingredients, a liquid telogen, an organometal initiator and a gaseous taxogen, and wherein the reactions which occur in said process comprise (a) chain transfer or transmetalation and (b) polymerization, and wherein the steps in which said (a) and (b) reactions were carried out are isolated to a substantial extent, the steps which comprise forming a solution of said initiator and said telogen whereby initially to metalate the telogen, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of the gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution in said first reaction zone, continuously passing the resulting intermixture containing telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing gaseous 1,3-butadiene through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer.
Claim 22
Dependent Claim
179 words
In a continuous process of producing normally liquid telomers in which there are interacted, as essential ingredients, a liquid telogen, an organometal initiator and a gaseous taxogen, and wherein the reactions which occur in said process comprise (a) chain transfer or transmetalation and (b) polymerization, and wherein the steps in which said (a) and (b) reactions were carried out are isolated to a substantial extent, the steps which comprise forming a solution of said initiator and said telogen whereby initially to metalate the telogen, continuously passing said solution to a first reaction zone in a first reactor vessel, continuously passing a controlled stream of the gaseous taxogen through fine apertures into said first reaction zone into direct contact with said initiator solution in said first reaction zone, continuously passing the resulting intermixture containing telomer through said reactor and into a second reaction zone in a second reactor vessel while continuously passing gaseous 1,3-butadiene through fine apertures into said second reaction zone into direct contact with said reaction intermixture produced in said first reactor to produce additional quantities of telomer.
Claim 23
Dependent Claim
51 words
The process of claim 18, wherein during passage through said first reactor after contact of the metalated liquid telogen with the gaseous taxogen polymerization of said taxogen occurs, and wherein, prior to passage of said intermixture into said second reactor, remetalation occurs of the liquid telomer which has previously been formed.
Claim 24
Dependent Claim
26 words
The process of claim 19, in which the telogen comprises toluene, the taxogen comprises 1,3-butadiene, and the initiator is a complex of n-butyllithium and potassium t-butoxide.
Claim 25
Dependent Claim
25 words
The process of claim 19, in which the telogen comprises toluene, the taxogen comprises 1,3-butadiene, and the initiator is a complex of n-butyllithium and N,N,N,',N'-tetramethylethylenediamine.
Claim 26
Dependent Claim
25 words
The process of claim 19, in which the telogen comprises toluene, the taxogen comprises 1,3-butadiene, and the initiator is a complex of dilithiodiisoprene and N,N,N',N'-tetramethylethylenediamine.
Claim 27
Dependent Claim
36 words
A telomer according to claim 2, in which the viscosity of the liquid telomer prepared by the continuous process is from about one-tenth to about one-half that of the liquid telomer prepared by the batch process.
Claim 28
Dependent Claim
37 words
A telomer according to claim 2, in which the volatiles content of the liquid telomer prepared by the continuous process is from about one-tenth to about one-half that of the liquid telomer prepared by the batch process.
Claim 29
Dependent Claim
40 words
A telomer according to claim 2, in which the molecular weight distribution of the liquid telomer prepared by the continuous process is from about 10 to about 35% lower than that of the liquid telomer prepared by the batch process.
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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) | 1980-09-19 | 1981-03-21 | 1981-09-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-09-19 | 1985-03-21 | 1985-09-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-09-19 | 1989-03-21 | 1989-09-20 | $7700.00 | Window Closed / Lapsed |