Process for the production of high purity and ultrapure bisphenol-A

• US 5,648,561 A
• Filed: 10/11/1995
• Issued: 07/15/1997
• Est. Priority Date: 02/17/1993
• Status: Expired due to Fees

• Current Assignee: China Petrochemical Corporation, Tianjin University
• Original Assignee: China Petrochemical Corporation, Tianjin University
• Inventors: Yu, Shenbo, Tan, Qiu, Liu, Zongzhang, Qian, Shenghua, Zhang, Minhua, Li, Chuanzhao
• Primary Examiner(s): Shaver, Paul F.
• Application Number:
  US08/505,309
• Time in Patent Office: 643 Days
• Field of Search: 568/724, 568/727
• US Class Current: 568/727
• CPC Class Codes: C07C 37/20 using aldehydes or ketones
• CPC Class Codes: C07C 37/74 by distillation
• CPC Class Codes: C07C 37/84 by crystallisation
• CPC Class Codes: C07C 39/16 Bis-(hydroxyphenyl) alkanes; Tris-(hydroxyphenyl)alkanes
• CPC Class Codes: Y02P 20/52 using catalysts, e.g. selective catalysts

Abstract

High purity and ultrapure bisphenol A is prepared in a novel process.

Claims

1. A process for the production of bisphenol-A comprising the steps of (1) reacting excess phenol and acetone in the presence of catalyst, (2) cooling the reaction mixture to form adduct crystals of bisphenol-A with phenol and a first mother liquor, (3) separating the adduct crystals from the first mother liquor and (4) removing phenol from the adduct crystals

wherein in step (1), excess phenol is reacted with acetone in a substantially vertical, multiple stage suspended reactive stripping apparatus comprising

(i) a reactor column which includes a side wall and a bottom,

(ii) a plurality of perforated trays provided in the reactor column,

(iii) a first screen located on each tray,

(iv) a plurality of downcomers interconnecting the trays, each of the downcomers having a second screen connected to the top thereof, the second screen, a portion of each said downcomers, a portion of the side wall of the reactor column and one of the perforated trays with the first screen thereon in combination defining a catalyst chamber, and

(v) a modified strong acid ion-exchange resin catalyst in the form of particulate solid contained within the catalyst chamber, and

wherein all of the phenol necessary for the condensation reaction thereof with acetone is charged to the reactor column from above the uppermost tray, portions of all the required acetone are charged to the tray next to the uppermost tray and at least some of the lower trays, and an inert gaseous stream is upwardly passed through the catalyst chambers to form solid-liquid suspensions and to strip water from the reaction mixture.

2. A process for the production of bisphenol-A according to claim 1 wherein in step (2), the liquid condensation reaction mixture effluent from the reactive stripping apparatus is cooled in a crystallizer to form a slurry containing crystals of the adduct of bisphenol-A and phenol and the mother liquor, said crystallizer having two filter means provided therein whereby a portion of the slurry containing fine adduct crystals of bisphenol-A and phenol having a particle size less than that of a predetermined crystalcut is allowed to pass alternatively through one of the filter means with a circulating pump and is then introduced into at least one fine crystal destructor from which a solution obtained after destruction of fine crystals is returned to the crystallizer through the other filter means with said or another circulating pump.

3. A process for the production of bisphenol-A according to claim 1 wherein step (4) comprises removing phenol from the adduct crystals obtained in step (3) by introducing the adduct crystals into at least one of a vacuum dephenolizer and an inert gaseous flow dephenolizer, bringing the adduct crystals to a temperature below the melting point thereof in the vacuum or in the presence of the inert gaseous stream to decompose the crystals into a gas phase and a solid phase, withdrawing the gas phase and discharging the solid phase as a high purity bisphenol-A product.

4. A process for the production of bisphenol-A according to claim 1 wherein the process further includes the steps of (5) recrystallizing the high purity bisphenol-A crystals obtained in step (4) above in the presence of solvent in a recrystallizer, and (6) separating the recrystallized bisphenol-A from a second mother liquor to obtain an ultrapure bisphenol-A product.

5. A process for the production of bisphenol-A according to claim 1 wherein the column trays include at least one of sieve trays and float valve trays.

6. A process for the production of bisphenol-A according to claim 1 wherein the mesh of the screen placed on the trays is smaller than the particle size of the catalyst particles.

7. A process for the production of bisphenol-A according to claim 1 wherein the catalyst load for each tray provided in the reactor column is in the range of from about 3% to about 10% by volume of the total volume of the catalyst and the reaction mixture.

8. A process for the production of bisphenol-A according to claim 1 wherein the molar ratio of phenol to acetone which is fed to the reactive stripping apparatus is in the range of from about 4 to about 12.

9. A process for the production of bisphenol-A according to claim 1 wherein the molar ratio of phenol to acetone which is fed to the reactive stripping apparatus is in the range of from about 7 to about 12.

10. A process for the production of bisphenol-A according to claim 1 wherein the molar ratio of phenol to acetone which is fed to the reactive stripping apparatus is about 7.

11. A process for the production of bisphenol-A according to claim 1 wherein the reaction temperature is in the range of from about 60°

C. to about 130°

C.

12. A process for the production of bisphenol-A according to claim 1 wherein the reaction temperature is in the range of from about 80°

C. to about 100°

C.

13. A process for the production of bisphenol-A according to claim 1 wherein the residence time calculated on the basis of dry catalyst weight is in the range of from about 0.25 to about 2 hrs.

14. A process for the production of bisphenol-A according to claim 1 wherein the inert gaseous stream comprises nitrogen.

15. A process for the production of bisphenol-A according to claim 1 wherein the velocity of the inert gaseous stream is in the range of from about 0.006 to about 0.075 m/s.

16. A process for the production of bisphenol-A according to claim 1 wherein the inert gaseous stream is removed from the reactive stripping apparatus, water is separated from the inert gaseous stream and the dewatered inert gaseous stream is then recycled to the bottom of the reactor column.

17. A process for the production of bisphenol-A according to claim 1 wherein the condensation reaction mixture effluent from step (1) is directly cooled to precipitate bisphenol-A in the form of adduct crystals containing bisphenol-A and phenol in a 1:

1 molar ratio.

18. A process for the production of bisphenol-A according to claim 1 wherein the reaction mixture is cooled to more than about 40°

C. in step (2).

19. A process for the production of bisphenol-A according to claim 1 wherein the reaction mixture is cooled to about 42°

C. in step (2).

20. A process for the production of bisphenol-A according to claim 2 wherein phenol and acetone are fed to the reactive stripping apparatus in a phenol:

acetone molar ratio of from about 4;

1 to about 12;

1, reaction takes place at a temperature in the range of from about 60°

C. to about 130°

C., and step (4) includes introducing the adduct crystals to a vacuum or inert gaseous flow dephenolizer, bringing the adduct crystals to a temperature below the melting point to decompose the crystals into a gas phase and a solid phase, and discharging the solid phase as a high purity bisphenol-A product.

21. A process for the production of bisphenol-A according to claim 20 wherein the process further includes the steps of:

(5) recrystallizing the high purity bisphenol-A obtained in step (4) in the presence of a solvent, and

(6) separating the recrystallized bisphenol-A from a second mother liquor to obtain an ultrapure bisphenol-A product.

22. A process for the production of bisphenol-A, comprising:

reacting acetone and phenol to form a reaction mixture containing bisphenol-A and water, cooling the reaction mixture to form bisphenol-A-phenol adduct crystals and a mother liquor, separating the adduct crystals from the mother liquor and removing phenol from the adduct crystals to obtain bisphenol-A, wherein

the reaction of acetone and phenol is conducted in a reactor column having a plurality of perforated trays supporting a solid particulate catalyst, and

an inert gas is passed upwardly through the reactor column during reaction in order to agitate the catalyst particles while stripping water from the reaction mixture, thereby forming a reaction mixture effluent having a reduced water content.

23. A process for the production of bisphenol-A according to claim 22 wherein during the cooling step, the reaction mixture effluent is cooled in a crystallizer containing at least first and second filter means, a portion of the crystallized reaction mixture which has a particle size less than that of a predetermined crystalcut is pumped through the first filter means and is then introduced into a crystal destructor to obtain a dissolved solution which is then returned to the crystallizer through the second filter means, the direction of circulation through the filter means being reversed after a predetermined period of time in order that a portion of the crystallized reaction mixture is pumped through the second filter means before being introduced into the crystal destructor and is returned to the crystallizer through the first filter means.

24. A process for the production of bisphenol-A according to claim 22 wherein phenol is removed from the adduct crystals in at least one of a vacuum dephenolizer and a pneumatic dephenolizer having an inert gas flow.

25. A process for the production of bisphenol-A according to claim 23 wherein phenol is removed from the adduct crystals in at least one of a vacuum dephenolizer and a pneumatic dephenolizer having an inert gas flow.