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    1.
    发明专利
    未知

    公开(公告)号：DE1079620B

    公开(公告)日：1960-04-14

    申请号：DEST014542

    申请日：1958-12-08

    Applicant: STAMICARBON

    Inventor： SOETERBROEK JOHANNES CORNELIS ,  GRAFF RENIER JOZEF LAMBERTUS

    IPC: B01D9/00 ,  C07C51/43

    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.

    4.
    发明专利
    未知

    公开(公告)号：DE2809272A1

    公开(公告)日：1978-09-07

    申请号：DE2809272

    申请日：1978-03-03

    Applicant: STAMICARBON

    Inventor： GRAFF RENIER JOZEF LAMBERTUS

    IPC: C08F4/00 ,  C08F4/60 ,  C08F4/64 ,  C08F10/00

    Abstract: An improved process for polymerizing alpha -alkenes and using Ziegler-type catalyst compositions is described. The Ziegler-type catalyst composition comprises a component consisting of an organoaluminum compound, an organomagnesium compound and a titanium compound or their reaction products on an inorganic porous solid particulate carrier material, wherein the aluminum/magnesium/titanium components are distributed and absorbed onto the inorganic carrier material, in separate steps, with removal of solvent or diluent therein between whereby the final catalyst/carrier composition when used in the polymerization process produces solid particulate polymer products with narrow particle size distributions.

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