Patent GB-899771-A (GB)
Title: Method of crystallizing adipic acid
IPC: C07C51/43
Filed: 1958-12-08
Abstract: Adipic acid is crystallized from solution by first cooling the solution to at least 30 DEG C. by direct heat exchange and then further cooling by indirect heat exchange, the direct heat exchange being effected in one or more stages by admixing the solution with a recycled portion of the suspension resulting from the second cooling and/or with a portion of the mother liquor Z  remaining after removal of crystal product from non-recycled suspension resulting from the second cooling.  When the direct heat exchange is effected in more than one stage, the solution is preferably cooled to 35 DEG -70 DEG C. in the first stage.  The adipic acid may be formed by the oxidation of cyclohexanol in an excess of nitric acid.  The invention may be applied to crystallization of the adipic acid from the nitric acid or to recrystallization of the adipic acid from water.  In one embodiment (Fig. 1, not shown) a solution of adipic acid in nitric acid at 90 DEG C. is mixed with a recycled crystal suspension at 15 DEG C. in a first crystallizer to produce a crystal suspension at 45 DEG C. which is mixed with further recycled crystal suspension at 15 DEG C. in a second crystallizer to produce a crystal suspension at 20 DEG C. which is cooled to 15 DEG C. in an indirect heat exchanger and then passed in part to a centrifugal separator and in part to the first and second recrystallizers as recycle.  Part of the suspension from the second crystallizer may pass directly to the centrifuge.  In a second embodiment (Fig. 2, not shown) a solution of adipic acid in water at 90 DEG C. is mixed with recycled mother liquor at 12,5 DEG C. in a first crystallizer to produce a crystal suspension at 65 DEG C. which is mixed with recycled crystal suspension at 12,5 DEG C. to produce a crystal suspension at 15 DEG C. which is cooled to 12,5 DEG C. in an indirect heat exchanger and then passed in part to a centrifugal separator, and in part to the second recrystallizer as recycle, mother liquor from the centrifugal separator being passed to the first recrystallizer as recycle.  Specification 745,063 is referred to.ALSO:Adipic acid is crystallized from solution by first cooling the solution to at least 30 DEG C. by direct heat exchange and then further cooling by indirect heat exchange, the direct heat exchange being effected in one or more stages by admixing the solution with a recycled portion of the suspension resulting from the second cooling and/or with a portion of the mother liquor remaining after removal of crystal product from nonrecycled suspension resulting from the second cooling.  When the direct heat exchange is effected in more than one stage, the solution is preferably cooled to 35 DEG C.-70 DEG C. in the first stage.  The adipic acid may be formed by the oxidation of cyclohexanol in an excess of nitric acid. The invention may be applied to crystallization of the adipic acid from the nitric acid or recrystallation of the adipic acid from water.  In one embodiment (Fig. 1, not shown) a solution of adipic acid in nitric acid at 90 DEG C. is mixed with a recycled crystal suspension at 15 DEG C. in a first crystallizer to produce a crystal suspension at 45 DEG C. which is mixed with further recycled crystal suspension at 15 DEG C. in a second crystallizer to produce a crystal suspension at 20 DEG C. which is cooled to 15 DEG C. in an indirect heat exchanger and then passed in part to a centrifugal separator and in part to the first and second recrystallizers as recycle.  Part of the suspension from the second crystallizer may pass directly to the centrifuge.  In a second embodiment (Fig. 2, not shown) a solution of adipic acid in water at 90 DEG C. is mixed with recycled mother liquor at 12.5 DEG C. in a first crystallizer to produce a crystal suspension at 65 DEG C. which is mixed with recycled crystal suspension at 12.5 DEG C. to produce a crystal suspension at 15 DEG C. which is cooled to 12.5 DEG C. in an indirect heat exchanger and then passed in part to a centrifugal separator, and in part to the second recrystallizer as recycle, mother liquor from the centrifugal separator being passed to the first recrystallizer as recycle. Specification 745,063 is referred to.