Polymerization initiating system and method to produce highly reactive olefin functional polymers
US-9771442-B2 · Sep 26, 2017 · US
US11274166B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11274166-B2 |
| Application number | US-201816499946-A |
| Country | US |
| Kind code | B2 |
| Filing date | Apr 9, 2018 |
| Priority date | Apr 12, 2017 |
| Publication date | Mar 15, 2022 |
| Grant date | Mar 15, 2022 |
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The present disclosure relates to the field of rubbers. The halogenated isobutylene isoprene rubber is prepared by polymerizing isoprene monomer and isobutylene monomer, followed by halogenation using a halogenating agent. This process of the present disclosure is simple, energy efficient and economic.
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The invention claimed is: 1. A process for preparation of halogenated isobutylene isoprene rubber, said process comprising: a. polymerizing isoprene monomer in a first fluid medium with isobutylene monomer to obtain a first product mass comprising isobutylene isoprene rubber; b. quenching the polymerization by adding an alcohol to the first product mass to obtain a first resultant product mass; c. adding a second fluid medium to the first resultant product mass to obtain a second resultant product mass; d. adding water to the second resultant product mass with continuous stirring, and allowing the second resultant product mass to stand to obtain a biphasic mixture comprising an organic phase and an aqueous phase, wherein the organic phase comprises isobutylene isoprene rubber, the first fluid medium, unreacted isobutylene monomer, unreacted isoprene monomer, and the second fluid medium, and an aqueous phase comprises the alcohol; e. separating the organic phase from the biphasic mixture; f. fractionally distilling the separated organic phase to obtain a bottom fraction comprising the isobutylene isoprene rubber and the second fluid medium; g. adding a halogenating agent to the bottom fraction and agitating to obtain a second product mass containing crude mixture comprising halogenated isobutylene isoprene rubber; and h. subjecting the crude mixture to the step of washing, steam stripping, and drying to obtain halogenated isobutylene isoprene rubber. 2. The process as claimed in claim 1 , wherein the step of polymerization comprises: i. introducing isoprene monomer, and at least one first fluid medium in a reactor to obtain a first mass; ii. cooling the first mass to a predetermined low temperature to obtain a cooled first mass; and iii. introducing isobutylene monomer in the reactor and agitating the reaction mass while maintaining the predetermined low temperature to obtain a first product mass comprising isobutylene isoprene rubber. 3. The process as claimed in claim 1 , wherein step (a) is optionally carried out in the presence of a catalyst selected from the group consisting of diethylaluminum chloride and ethylaluminum dichloride. 4. The process as claimed in claim 1 , wherein the first fluid medium is at least one selected from the group consisting of ethyl chloride, isopentane, and hexane. 5. The process as claimed in claim 1 , wherein the alcohol is at least one selected from the group consisting of methanol and ethanol. 6. The process as claimed in claim 2 , wherein the predetermined low temperature is in the range of −40° C. to −80° C. 7. The process as claimed in claim 1 , wherein the second fluid medium is at least one selected from the group consisting of hexane and isopentane. 8. The process as claimed in claim 1 , wherein the step of fractional distillation is carried out at a temperature in the range of 30° C. to 150° C. and at a pressure in the range of 3 kg/cm to 8 kg/cm. 9. The process as claimed in claim 1 , wherein the halogenating agent is at least one selected from the group consisting of bromine (Br 2 ) and chlorine gas. 10. The process as claimed in claim 1 , wherein the step of washing is carried out with at least one aqueous alkali selected from the group consisting of sodium hydroxide, potassium hydroxide, and sodium bishulphide.
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