Patent US3852253A successfully refreshed from Google Patents.
US3852253A
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Heterogeneous process for preparing conjugated diene butyl
Assignee: ExxonMobil Technology and Engineering Co
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Filing: 1972-12-22
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Granted: 1974-12-03
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Expires: 1992-12-22
Abstract
Abstract Dehydrohalogenation of halogenated butyl rubber to produce a butyl rubber having conjugated double bonds, a major portion of which are in the linear backbone. The process produces a composition having the schematic formula: WHERE N + 1 REPRESENT THE NUMBER OF ISOOLEFIN UNITS INCORPORATED IN THE BUTYL RUBBER POLYMER BACKBONE, AND M REPRESENTS THE NUMBER OF CONJUGATED DIOLEFIN UNITS PRESENT, SUBSTANTIALLY AS RANDOMLY INSERTED UNITS. The process for preparing the above compositions comprises contacting a solution of halogenated butyl rubber with a strong mineral acid salt of a metal selected from the metals of Groups IIa and IIb of the Periodic Table. Both brominated and chlorinated butyl rubber may be used in the present process to produce a butyl rubber having greater than about 0.4 mole percent conjugated diene unsaturation present in the polymer.
Inventors
- 👤 A Malatesta
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 23:43
CPC Classifications
C; C08; C08F; C08F8/00; C08F8/26
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
164 words
A HETEROGENEOUS PROCESS FOR PREPARING A COPOLYMER CONSISTING OF FROM 85 TO 99.5 PER CENT BY WEIGHT OF AN ISOOLEFIN HAVING FROM 4 TO 7 CARBON ATOMS, COMBINED WITH 15 TO 0.5 PERCENT BY WEIGHT OF A CONJUGATED DIOLEFIN HAVING FROM 4 TO 14 CARBON ATOMS, CONTAINING IN THE LINEAR BACKBONE CONJUGATED DIENE UNSATURATION WHICH COMPRISES CONTACTING A SLOUTION OF SAID COPOLUMER WHICH HAS BEEN HALOGENATED, IN A REACTION ZONR WITH A METAL SALT OF A STRONG ACID WHEREIN SAID METAL SI SELECTED FROM THE METALS OF GROUP IIA OR IIB OF THE PERIODIC TABLE; PROVIDED, HOWEVER, THAT SAID SALT IS NOT A FRIEDEL-CRAFTS CATALYST, THERE BEING AT LEAST 1 PART BY WEIGHT SALT PRESENT FOR CONTACT WITH 100 PARTS BY WEIGHT OF SAID HALOGENATED COPOLYMER, AT A TEMPERATURE OF FROM 100* TO 220*C., FOR A TIME SUFFICIENT TO DEHYDEOHALOGENATED SAID HALOGENATED COPOLYMER, AND RECOVERING THE COPOLYMER HAVING A REDUCED HALOGEN CONTENT , WHICH IS CHARACTERIZED BY HAVING RANDOM UNITS OF CONJUGATED DIENE UNSATURATION.
Claim 2
Dependent Claim
164 words
A HETEROGENEOUS PROCESS FOR PREPARING A COPOLYMER CONSISTING OF FROM 85 TO 99.5 PER CENT BY WEIGHT OF AN ISOOLEFIN HAVING FROM 4 TO 7 CARBON ATOMS, COMBINED WITH 15 TO 0.5 PERCENT BY WEIGHT OF A CONJUGATED DIOLEFIN HAVING FROM 4 TO 14 CARBON ATOMS, CONTAINING IN THE LINEAR BACKBONE CONJUGATED DIENE UNSATURATION WHICH COMPRISES CONTACTING A SLOUTION OF SAID COPOLUMER WHICH HAS BEEN HALOGENATED, IN A REACTION ZONR WITH A METAL SALT OF A STRONG ACID WHEREIN SAID METAL SI SELECTED FROM THE METALS OF GROUP IIA OR IIB OF THE PERIODIC TABLE; PROVIDED, HOWEVER, THAT SAID SALT IS NOT A FRIEDEL-CRAFTS CATALYST, THERE BEING AT LEAST 1 PART BY WEIGHT SALT PRESENT FOR CONTACT WITH 100 PARTS BY WEIGHT OF SAID HALOGENATED COPOLYMER, AT A TEMPERATURE OF FROM 100* TO 220*C., FOR A TIME SUFFICIENT TO DEHYDEOHALOGENATED SAID HALOGENATED COPOLYMER, AND RECOVERING THE COPOLYMER HAVING A REDUCED HALOGEN CONTENT , WHICH IS CHARACTERIZED BY HAVING RANDOM UNITS OF CONJUGATED DIENE UNSATURATION.
Claim 3
Dependent Claim
153 words
A heterogeneous process for dehydrohalogenating a halogenated copolymer consisting of from 85 to 99.5 percent by weight isobutylene, combined with 15 to 0.5 percent by weight isoprene, having a number average molecular weight of about 5,000 to 500, 000 to form the dehydrohalogenated copolymer characterized by having random units of conjugated diene unsaturation comprising contacting a solution of halogenated copolymer, in a reaction zone with a hydrocarbon insoluble metal salt of a strong acid wherein the metal is selected from the metals of Group IIa or IIb, at a temperature of from 130* to 180*C., there being at least from 1 to 10 parts by weight salt in contact with 100 parts of said halogenated copolymer, and said metal salt not being a Friedel-Crafts catalyst, said contact of metal salt with the halogenated copolymer being for A time sufficient to dehydrohalogenate the halogenated copolymer, and recovering said copolymer having a reduced halogen content.
Claim 4
Dependent Claim
153 words
A heterogeneous process for dehydrohalogenating a halogenated copolymer consisting of from 85 to 99.5 percent by weight isobutylene, combined with 15 to 0.5 percent by weight isoprene, having a number average molecular weight of about 5,000 to 500, 000 to form the dehydrohalogenated copolymer characterized by having random units of conjugated diene unsaturation comprising contacting a solution of halogenated copolymer, in a reaction zone with a hydrocarbon insoluble metal salt of a strong acid wherein the metal is selected from the metals of Group IIa or IIb, at a temperature of from 130* to 180*C., there being at least from 1 to 10 parts by weight salt in contact with 100 parts of said halogenated copolymer, and said metal salt not being a Friedel-Crafts catalyst, said contact of metal salt with the halogenated copolymer being for A time sufficient to dehydrohalogenate the halogenated copolymer, and recovering said copolymer having a reduced halogen content.
Claim 5
Dependent Claim
55 words
The heterogeneous process of claim 1, wherein the catalyst is a metal salt of a strong acid wherein the metal salt is a phosphate, sulfate, chloride and nitrate, of a metal selected from the metals of Groups IIa and IIb of the Periodic Table; provided, however, that the metal salt is not a Friedel-Crafts catalyst.
Claim 6
Dependent Claim
13 words
The heterogeneous process of claim 3, wherein the Group IIa metal is calcium.
Claim 7
Dependent Claim
23 words
The heterogeneous process of claim 3, wherein the Group IIb metal is zinc, and further wherein said catalyst is not a Friedel-Crafts catalyst.
Claim 8
Dependent Claim
12 words
The heterogeneous process of claim 1, wherein said catalyst is tricalcium orthophosphate.
Claim 9
Dependent Claim
12 words
The heterogeneous process of claim 1, wherein said catalyst is zinc orthophosphate.
Claim 10
Dependent Claim
12 words
The heterogeneous process of claim 1, wherein said catalyst is calcium sulfate.
Claim 11
Dependent Claim
12 words
The heterogeneous process of claim 1, wherein said catalyst is calcium chloride.
Claim 12
Dependent Claim
42 words
The heterogeneous process of claim 1, wherein the solution of halogenated butyl rubber is contacted with the strong acid salt of a Group IIa or IIb metal in a reaction zone characterized by having a fixed bed of said metal salt catalyst.
Claim 13
Dependent Claim
36 words
The heterogeneous process of claim 1, wherein the solution of halogenated butyl rubber is contacted with the strong acid salt of a Group IIa or IIb metal suspended in the reaction medium in stirred reaction zone.
References Cited (Backward Citations)
US3084142A
Cited
US3646166A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-12-02 | 1978-06-03 | 1978-12-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-12-02 | 1982-06-03 | 1982-12-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-12-02 | 1986-06-03 | 1986-12-03 | $7700.00 | Window Closed / Lapsed |