Countercurrent multi-stage water crystallization of aromatic compounds

• US 4,861,919 A
• Filed: 02/29/1988
• Issued: 08/29/1989
• Est. Priority Date: 02/29/1988
• Status: Expired due to Term

• Current Assignee: Diamond Technology Partnership Company
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Gammill, Ben B., Robbins, Lanny A.
• Primary Examiner(s): Lee, Mary C.
• Assistant Examiner(s): Howard, MarySue
• Application Number:
  US07/161,589
• Time in Patent Office: 547 Days
• Field of Search: 260/707, 568/724
• US Class Current: 568/724
• CPC Class Codes: C07C 37/685 Processes comprising at least two steps in series
• CPC Class Codes: C07C 37/84 by crystallisation
• CPC Class Codes: C07C 39/16 Bis-(hydroxyphenyl) alkanes; Tris-(hydroxyphenyl)alkanes

Abstract

A process for the purification of an aromatic compound, e.g. isopropylidenediphenol, comprising using a multi-stage countercurrent process wherein the crystals are melted by the addition of heat and water prior to each crystallization step and wherein one crystallization is accomplished at a pre-selected low temperature.

Claims

1. A multi-stage, countercurrent process for the removal of impurities from a mixture of bisphenol-A and congeneric impurities contaminated by one or more related congeneric impurities, the process comprising subjecting the crude compound to at least two cycles of crystallization and purification wherein the purification step(s) comprise washing the crystals of the bisphenol-A countercurrently with a mixture of the compound in molten form and water followed by a final crystallization step wherein the cycles comprise

(1) melting the compound crystals prior to each crystallization by the addition of heat and water and in the absence of an added organic solvent;

(2) conducting one crystallization step at a low temperature pre-selected to increase recovery of the bisphenol-A;

(3) conducting at least one crystallization step at a temperature greater than about 95°

C.; and

(4) separating water and oil which remain after each of the purification steps of the process and after the final crystallization step; and

(a) recycling the separated water to the crystallization and purification step(s); and

(b) recycling the separated oil to be recrystallized;

and the final crystallization step consists essentially of separating the crystals from the oil and water and drying the crystals without further purification.

2. The process of claim 1 wherein the pre-selected low temperature is 70°

0 C.

3. The process of claim 2 wherein the p,p'"'"'-isopropylidenediphenol obtained is at least about 99.99 percent pure.

4. The process of claim 3 wherein the p,p'"'"'-isopropylidenediphenol is obtained in a yield of at least about 98 percent based on the amount of crude p-bisphenol provided.

5. The process of claim 1 comprising subjecting the crude bisphenol-A to two cycles of crystallization and purification followed by a final crystallization step.

6. The process of claim 1 wherein the pre-selected low temperature is the lowest temperature at which the bisphenol-A will crystallize out of a eutectic mixture of the bisphenol-A and its related impurities.

7. The process of claim 1 wherein the purification step is accomplished using a counter-current wash column equipped with a heater and a water inlet.

8. The process of claim 1 wherein the crystallization step(s) is(are) accomplished using an adiabatic, evaporatively cooled, mixed suspension crystallizer(s).