Continuous process for preparation of dian

• US 4,301,305 A
• Filed: 12/28/1979
• Issued: 11/17/1981
• Est. Priority Date: 12/30/1978
• Status: Expired due to Term

• Current Assignee: Instytut Ciezkiej Syntezy Organicznej "Blachownia"
• Original Assignee: Instytut Ciezkiej Syntezy Organicznej "Blachownia"
• Inventors: Grzywa, Edward, Kolt, Jozef, Terelak, Kazimierz, Czyz, Jerzy, Kiedik, Maciej, Niezgoda, Anna
• Primary Examiner(s): LONE, WERREN
• Application Number:
  US06/108,403
• Time in Patent Office: 690 Days
• Field of Search: 568/727, 568/728, 568/788
• US Class Current: 568/727
• CPC Class Codes: B01J 2208/00274 involving reactant vapours
• CPC Class Codes: B01J 8/006 by filtration
• CPC Class Codes: B01J 8/0449 in two or more cylindrical beds
• CPC Class Codes: B01J 8/0457 the beds being placed in separate reactors
• CPC Class Codes: C07C 37/20 using aldehydes or ketones
• CPC Class Codes: C07C 39/16 Bis-(hydroxyphenyl) alkanes; Tris-(hydroxyphenyl)alkanes

Abstract

The dian is prepared by the condensation of phenol with acetone in the presence of acid ion-exchange catalyst of the type of sulfonated co-polymer of styrene and divinylbenzene. The three-stage process is conducted in two reactors packed with a stationary catalyst bed. In each of the reactors the bed height is 5-20 m and in addition, in both reactors the beds are divided into bottom and upper zones.

At various stages of the process, a reaction mixture is circulated with a different linear velocity, the first step of the process being conducted at a temperature of 60°-85° C. in the bed of the first reactor, in succession in the bottom and then upper zone of the catalytic bed; the second stage of the process is accomplished in the bottom zone of the second reactor at a temperature of 70°-90° C.; and the third step is carried out in the upper zone of the second reactor at a temperature of 75°-95° C.

The linear velocity of the reaction mixture flow through the bottom zones of the bed is not greater than 10 m/h, and the linear velocity of flow through the upper zones of the reactor bed is not higher than 4 m/h.

The sequence of the reaction mixture flow through the reactors is being changed in cycles, and at interstage intervals the reaction mixture is filtered to separate minus mesh and comminuted particles of the catalyst.

Claims

1. A method of preparing dian by condensation of phenol with acetone in the presence of acid ion-exchange catalyst of sulfonated copolymer of styrene and divinylbenzene, with multiple circulation of the reaction mixture through a catalyst bed, wherein said process is conducted in three stages, characterized in that said three stages of the process are performed in two reactors in two stationary catalyst beds, each of the beds having a height of 5-20 m, each of said beds being divided into an upper and bottom zone;

wherein said reaction mixture is circulated in particular stages of the process with a different linear velocity, said first stage of the process being conducted in the bed of the first reactor in turn in said bottom and then upper zone of the catalytic bed at a temperature of 80°

-85°

C., said second stage being carried out in the bottom zone of the catalytic bed of the second reactor at a temperature of 65°

C. to 90°

C., and the third stage of the process being conducted in the upper zone of the second reactor at a temperature of 70°

to 95°

C., wherein said linear velocity of flow of the reaction mixture through the bottom zones of the catalytic bed in both of the reactors is not greater than 10 m/h, and the linear velocity of flow of the reaction mixture through the upper zones of the catalyst bed in both of the reactors is not greater than 4 m/h.

2. The method of claim 1 wherein the sequence of flow of said reaction mixture through the catalyst beds in both of the reactors is changed in cycles.

3. The method of claims 1 and 2 wherein at least a portion of said reaction mixture is passed by filter to remove undersize and comminuted particles of the catalyst.

4. The method of claim 1 wherein a boundary of the bed divided into the upper and bottom zones in the reactors is defined by a system of injection-filtration nozzles said nozzles supplying the catalyst bed with the reaction mixture or withdrawing said mixture from the bed.