Three phase crystallization

• US 4,141,924 A
• Filed: 11/11/1977
• Issued: 02/27/1979
• Est. Priority Date: 01/27/1969
• Status: Expired due to Term

• Current Assignee: The Dow Chemical Company (Dow, Inc.)
• Original Assignee: The Dow Chemical Company (Dow, Inc.)
• Inventors: Sun, Yun C.
• Primary Examiner(s): Davis, C.
• Application Number:
  US05/850,512
• Time in Patent Office: 473 Days
• Field of Search: 260/674 R, 260/674 A, 260/674 N, 62/532
• US Class Current: 585/817
• CPC Class Codes: C07C 15/08 Xylenes
• CPC Class Codes: C07C 15/14 all phenyl groups being directly linked
• CPC Class Codes: C07C 15/24 containing two rings
• CPC Class Codes: C07C 37/84 by crystallisation
• CPC Class Codes: C07C 39/16 Bis-(hydroxyphenyl) alkanes; Tris-(hydroxyphenyl)alkanes
• CPC Class Codes: C07C 7/14 by crystallisation; Purification or separation of the crystals

Abstract

A process for purifying a crude crystalline or crystallizable water-immiscible aromatic compound contaminated with one or more related congeneric impurities which cannot be readily separated by distillation, said process comprising:

(1) forming a dispersion of liquefied crude material in an aqueous liquid by agitating the mixture;

(2) effecting crystallization of the desired aromatic compound while maintaining the dispersion;

(3) reducing agitation sufficiently to permit the formation of three phases, i.e., a solid crystalline phase, an aqueous liquid phase, and a mother liquor phase; and

(4) separating the crystals;

Said aqueous liquid being immiscible with, and having a density between, the aforementioned solid crystalline phase and the mother liquor phase.

Claims

1. A process for purifying a crude aromatic hydrocarbon having 1 to 3 rings and the alkyl substituted derivatives thereof from a mixture containing at least 25 weight percent of said compound, contaminated with one or more related congeneric impurities which cannot be readily separated by distillation, said process comprising:

(1) forming a dispersion of the liquefied crude aromatic hydrocarbon, said liquefaction being the result of melting or solvent solution, in an immiscible aqueous 20% solution of an inert compound selected from the group consisting of NaCl, NH₃, CaCl₂, (NH₄)₂ SO₄, or (NH₄)₃ PO₄ by agitating a mixture of the two wherein said aqueous liquid is substantially immiscible with both (a) the aromatic hydrocarbon, and (b) the mother liquor phase composed of the liquid impurities and solvent, if any, containing the liquid impurities, and the said aqueous liquid has a density between (a) and (b),

(2) effecting crystallization of the aromatic hydrocarbon to be purified while maintaining the dispersion;

(3) centrifuging the mixture to permit the formation of three phases, i.e., a solid crystalline phase, an aqueous liquid phase, and a mother liquor phase, said aqueous liquid phase having sufficient height to completely separate the crystalline and mother liquor phases; and

(4) separating the crystals from step (3) without contact between the crystals and mother liquor.

2. The process of claim 1 wherein the compound to be purified is biphenyl.

3. The process of claim 1 wherein the compound to be purified is naphthalene.

4. The process of claim 1 wherein the compound to be purified is p-xylene.