Abstract:
IMPROVEMENT IN OR MODIFICATION OF THE PROCESS DESCRIBED IN COPENDING APPLICATION SER. NO. 587,434, NOW U.S. PAT. NO. 3,413,365 COMPRISING WITHDRAWING RESULTING DICHLOROBUTENE MIXTURE AT A REFLUX RATION OF R=1 TO 20; WITHDRAWING THE COMPLETELY CONDENSED MATTER OR REFLUX MATTER NEAR THE COLUMN BASE; INTRODUCING SUCH MATTER INTO A CIRCULATION EVAPORATOR AND RECYCLING IT LATER IN VAPOR FORM FROM SAID EVAPORATOR INTO THE REACTOR; CONTINUOUSLY SUPPLYING THE SAID CIRCULATION EVAPORATOR WITH METERED QUANTITIES OF FRESH TETRACHLOROBUTANE-CONTAINING 1,2,3-TRICHLOROBUTANE COMING FROM A RSERVOIR, THE SAID TETRACHLOROBUTANECONTAINING 1,2,3-TRICHLOROBUTANE BEING SUPPLIED AT THE SAME RATE AS PRODUCED DICHLOROBUTENE MIXTURE IS WITHDRAWN FROM THE COLUMN; AND, ONCE THE 1,2,3-TRICHLOROBUTANE IN THE REACTOR IS FOUND TO CONTAIN ABOUT 30% BY WEIGHT TETRACHLOROBUTANE, INTRODUCING A PORTION OF THE REFLUX MATTER WITHDRAWN NEAR THE COLUMN BASE INTO A STIRRABLE COOLER; CENTRIFUGING THE 2,2,3,3-TETRACHLOROBUTANE, WHICH IS FOUND PARTIALLY TO CRYSTALLIZE IN THE SAID COOLER AT A TEMPERATURE OF 0*C., AND WITHDRAWING IT; AND RECYCLING MOTHER LIQUOR TO THE SAID CIRCULATION EVAPORATOR.