Claims
- 1. A catalytic process for the manufacture of 1,4-bis(4-phenoxybenzoyl)benzene, said process comprising contacting diphenyl ether for a period of about 40-360 min at a temperature of about 190.degree.-250.degree. C. with 1,4-benzenedicarbonyl chloride in the presence of a zeolite selected from the group consisting of:
- (a) activated zeolites in hydrogen-exchanged form having a ring structure containing 12 oxygen atoms and belonging to one of the classes of naturally occurring faujasites, naturally occurring mordenites, synthetic zeolites Y, and synthetic mordenites, and
- (b) iron-exchanged zeolites having a ring structure containing 12 oxygen atoms and belonging to one of the classes of naturally occurring faujasites, naturally occurring mordenites, synthetic zeolites X and Y, and synthetic mordenites,
- the weight ratio of 1,4-benzenedicarbonyl chloride to hydrogen-exchanged zeolite being about 3:1 to 1:2, and to iron-exchanged zeolite about 10:1 to 1:2, and the mole ratio of diphenyl ether to 1,4-benzenedicarbonyl chloride being about 15-80:1, when a hydrogen-exchanged zeolite is the catalyst and about 10-50:1 when an iron-exchanged zeolite is the catalyst,
- separating the zeolite from the resulting hot solution, cooling the hot solution to a temperature at which BPBB crystallizes, and separating the crystalline product from the cooled solution.
- 2. A process of claim 1, paragraph (a), wherein the mole ratio of diphenyl ether to 1,4-benzenedicarbonyl chloride is about 40-50:1.
- 3. A process of claim 1, paragraph (b), wherein the mole ratio of diphenyl ether to 1,4-benzenedicarbonyl chloride is about 15-20:1.
- 4. A process of claim 1 wherein the reaction temperature is held with the range of about 220.degree.-250.degree. C.
- 5. A process of claim 4 wherein the reaction time is about 60-150 minutes.
- 6. A process of claim 5, wherein the reaction temperature is about 250.degree. C., and the reaction time is about 120 min.
- 7. A process of claim 1 wherein the solution remaining after the removal of the zeolite catalyst is cooled to about 25.degree.-40.degree. C. prior to the recovery of the crystalline product.
- 8. A process of claim 1 which is conducted at atmospheric pressure.
- 9. A process of claim 1 which is conducted at a reduced pressure.
- 10. A process of claim 9 which is conducted at a pressure at which diphenyl ether is refluxing.
- 11. A process of claim 1 which is a batch process.
- 12. A process of claim 11, in which an iron-exchanged zeolite catalyst is used repeatedly in successive batches.
- 13. A process of claim 1 which is a continuous process.
- 14. A process of claim 1 wherein the zeolite catalyst is a reused, hydrogen-exchanged regenerated catalyst which has been earlier used according to the process of claim 1.
- 15. A process of claim 1 wherein the catalyst is an iron-exchanged zeolite, which is calcined prior to use and heated in air for several hours.
- 16. A process of claim 1 wherein the catalyst is an iron-exchanged zeolite, which is heated for several hours prior to use in the presence of hydrogen chloride.
CROSS-REFERENCE TO RELATED APPLICATION
This is a continuation-in-part of our copending application Ser. No. 07/117,991, filed Nov. 9, 1987 now abandoned.
US Referenced Citations (12)
Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
117991 |
Nov 1987 |
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