Process for the production of terephthalic acid

Abstract

Terephthalic acid is produced by oxidation of para xylene, purified in an aqueous phase and recovered by precipitating a purified product from the aqueous phase, the aqueous phase mother liquor is then cooled or evaporated to produce a further less pure precipitate and a second mother liquor and the less pure precipitate is returned to the reaction medium and/or the water of the second mother liquor is used to dissolve the crude solid and/or the second mother liquor is treated to recover water which is used to wash the precipitate recovered from the aqueous solution. The process produces better yields of terephthalic acid, reduces the use of water and reduces problems in the disposal of polluted waste water.

We claim: 
     
       1. A process in which terephthalic acid is produced of oxidizing para xylene to terephthalic acid in a liquid reaction medium which comprises acetic acid and in which terephthalic acid is separated from the liquid reaction medium as a crude solid, dissolved in a liquid comprising water to produce a solution and purified by a process which comprises contacting the solution under reducing conditions with hydrogen and a heterogenous catalyst for the reduction of at least some impurities, the solution is cooled after said reduction to precipitate solid purified terephthalic acid, aqueous mother liquor is separated from the precipitate wherein; a) the aqueous mother liquor is treated to produce a less pure precipitate comprising terephthalic acid and a second mother liquor;   b) the less pure precipitate is returned directly or indirectly to the reaction medium; and   c) at least part of the said second mother liquor is, directly as such or indirectly after treatment, used to dissolve the crude solid.   
     
     
       2. A process in which terephthalic acid is produced by oxidizing para xylene to terephthalic acid in a liquid reaction medium which comprises acetic acid and in which terephthalic acid is separated from the liquid reaction medium as a crude solid, dissolved in a liquid comprising water to produce a solution and purified by a process which comprises contacting the solution under reducing conditions with hydrogen and a heterogenous catalyst for the reduction of at least some impurities, the solution is cooled after said reduction to precipitate solid purified terephthalic acid, aqueous mother liquor is separated from the precipitate wherein; a) the aqueous mother liquor is treated to produce a less pure precipitate comprising terephthalic acid and a second mother liquor;   b) the less pure precipitate is returned directly or indirectly to the reaction medium;   c) at least part of the second mother liquor is subjected to fractional distillation to recover water from the second mother liquor; and   d) the recovered water is used to wash the precipitate recovered from said solution after the reduction step.   
     
     
       3. A process according to claims . .1 or 2.!. .Iadd.1, 2, 9 or 10 .Iaddend.in which, . .in step a).!., .Iadd.in the step to produce a less pure precipitate .Iaddend.the mother liquor is cooled to a temperature within the range of 15° to 100° C. to produce said less pure precipitate. 
     
     
       4. A process according to claim 2 in which the fractional distillation (c) is carried out in a column at a reflux ratio of 2 to 10. 
     
     
       5. A process according to claim 4 in which 25 to 125 theoretical plates are used. 
     
     
       6. A process according to claim 4 in which the mother liquor returned to the fractional distillation is fed at within 0 to 30% of the theoretical plates from the top of the column. 
     
     
       7. A process according to . .claim 1 or 2.!. .Iadd.claims 1, 2, 9 or 10 .Iaddend.in which the precipitation step to produce . .pure.!. .Iadd.purified .Iaddend.terephthalic acid is operated at a pressure of at least 3 bar. 
     
     
       8. A process according to claims . .1 or 2.!. .Iadd.1, 2, 9 or 10 .Iaddend.in which, . .in step a).!. .Iadd.in the step to produce a less pure precipitate, .Iaddend.the mother liquor is cooled to produce said less pure precipitate. .Iadd. 
     
     
       9.  A process for the production of terephthalic acid comprising: in a first reactor oxidizing para xylene to terephthalic acid in a liquid reaction medium which comprises acetic acid, the reaction being accompanied by the evolution of vapor comprising acetic acid and water;   condensing said vapor and passing part of the condensate to a distillation column for separating acetic acid and water;   separating terephthalic acid from the liquid reaction medium as a crude solid;   dissolving the crude terephthalic acid in a liquid comprising water to produce a solution;   in a second reactor contacting the solution under reducing conditions with hydrogen and a heterogeneous catalyst for the reduction of at least some impurities;   cooling the solution after said reduction to precipitate solid purified terephthalic acid;   separating primary aqueous mother liquor from the precipitate;   treating the primary aqueous mother liquor to produce a less pure precipitate comprising terephthalic acid and a secondary mother liquor containing dissolved contaminants including p-toluic acid;   passing at least part of the secondary mother liquor to said distillation column for the separation of acetic acid from water;   operating the distillation column to produce a bottom product containing acetic acid from said condensate together with p-toluic acid and other high boiling point contaminants present in the secondary mother liquor and an overhead product comprising water derived from said condensate and said secondary mother liquor; and   supplying said bottom product to the first reactor..Iaddend..Iadd.   
     
     
       10.  A process as claimed in claim 9 further comprising returning the less pure precipitate directly or indirectly to the reaction medium..Iaddend..Iadd.11. A process as claimed in claim 9 or 10 comprising using at least part of the water derived from the distillation column to wash said precipitate comprising purified solid terephthalic acid..Iaddend..Iadd.12. A process as claimed in claim 9 or 10 comprising using at least part of the water derived from the distillation column in the dissolution of the crude terephthalic acid to produce said 
     
     
        solution..Iaddend..Iadd.13.  A process as claimed in claim 9 in which said distillation is carried out in a column at a reflux ratio of 20 to 10..Iaddend..Iadd.14. A process as claimed in claim 13 in which 25 to 125 theoretical plates are used in said distillation..Iaddend..Iadd.15. A process as claimed in claim 13 or 14 in which the secondary mother liquor is fed at within 0 to 30% of the theoretical plates from the top of the column..Iaddend.