公开(公告)号：US3850981A

公开(公告)日：1974-11-26

申请号：US14360471

申请日：1971-05-14

Applicant: CELANESE CORP

Inventor： TREBELLAS J ,  THIGPEN H ,  MAYS W

IPC: C07C51/265 ,  C07C63/02

CPC classification number: C07C51/265 ,  C07C63/16 ,  C07C63/26 ,  C07C63/24

Abstract: 1. A CONTINUOUS PROCESS FOR THE LIQUID PHASE OXIDATION OF M-XYLENE OR P-XYLENE TO THE CORRESPONDING BENZENE DICARBOXYLIC ACID COMPRISING: (A) CONTINUOUSLY FEEDING M-XYLENE AND/OR P-XYLENE, ACETALDEHYDE, AN OXYGEN-CONTAINING GAS, ACETIC ACID AND A SOLUBLE COBALT SALT CATALYST TO A REACTOR HAVING A GAS PHASE AND A LIQUID-SOLID SLURRY PHASE, THE AMOUNT OF OXYGEN-CONTAINING GAS BEING SUFFICIENT TO PROVIDE AT LEAST 3.25 MOLES OXYGEN PER MOLE OF XYLENE, THE WEIGHT RATIO OF ACETALDEHYDE TO XYLENE BEING AT LEAST 0.2:1, THE WEIGHT RATIO OF ACETIC ACID TO XYLENE BEING FROM ABOUT 3:1 TO 15:1 AND THE AMOUNT OF CATALYST BEING SUFFICIENT FO PROVIDE ABOUT 0.1 TO 2.5% COBALT METAL BASED ON THE COMBIND WEIGHT OF XYLENE, ACETIC ACID AND ACETALDEHYDE, (B) MAINTAINING BACKMIXING CONDITIONS IN THE LIQUIDSOLID SLURRY PHASE OF SAID REACTOR, MAINTAINING IN SAID REACTOR A STEADY STATE CONCENTRATION OF AROMATIC BENZENE DICARBOXYLIC ACID PRECURSORS OF LESS THAN 3% BY WEIGHT OF THE LIQUID-SOLID SLURRY PHASE PRESENT, A TEMPERATURE OF FROM 120-140*C., A PRESSURE OF AT LEAST 95 P.S.I.G., AND MAINTAINING THE AVERAGE RESIDENCE TIME OF THE REACTANTS IN THE REACTOR SUCH THAT AT LEAST 98.6% OF THE XYLENE FED IS CONVERTED TO SOME OTHER PRODUCT AND (C) CONTINUOUSLY WITHDRAWING FORM SAID REACTOR A PORTION OF THE LIQUID-SOLID SLURRY PHASE AND A PORTION OF THE GASEOUS PHASE AND RECOVERING TEREPHTHALIC ACID FROM SAID PORTION WITHDRAWN FROM SAID LIQUID-SOLID SLURRY PHASE.

公开(公告)号：US3840469A

公开(公告)日：1974-10-08

申请号：US27539572

申请日：1972-07-26

Applicant: CELANESE CORP

Inventor： HUGUET J ,  HOBBS C ,  TREBELLAS J

IPC: B01J31/04 ,  B01J31/40 ,  C01G51/00 ,  C07C51/215 ,  C22B3/16 ,  C22B3/32 ,  B01J11/02 ,  B01J11/82 ,  C07C53/08

CPC classification number: B01J31/403 ,  B01J31/04 ,  B01J31/2234 ,  B01J2231/70 ,  B01J2531/845 ,  C01G51/00 ,  C01P2002/54 ,  C07C51/215 ,  C22B3/0025 ,  C22B3/165 ,  Y02P10/234 ,  Y02P20/584

Abstract: 1. A PROCESS FOR THE RECOVERY OF COBALT (II) IONS INITIALLY PRESENT IN A FIRST LIQUID MEDIUM CONSISTING ESSENTIALLY OF ACETIC ACID DERIVED FROM THE LIQUID PHASE OXIDATION OF AN ALIPHATIC HYDROCARBON AND THE PRODUCTION OF A FRESH SOLUTION OF THE SAME COMPRISING: (A) INCORPORATING INTO SAID FIRST ACETIC MEDIUM CONTAINING COBALT (II) IONS AND ABOUT 3 TO 15 PERCENT WATER BY WEIGHT A SOURCE OF OXALATE IONS IN A QUANTITY AT LEAST SUFFICIENT TO REACT STOICHIOMETRICALLY WITH SAID COBALT (II) IONS TO FORM COBALT OXALATE (B) FORMING A SOLID PRECIPITATE OF COBALT 8II) OXALATE IN SAID FIRST ACETIC MEDIUM WHILE AT A TEMPERATURE OF ABOUT 20 TO 150*C., (C) SEPARATING SAID PRECIPITATE OF COBALT OXALATE FROM SAID FIRST ACETIC ACID MEDIUM (D) CONTACTING SAID SEPARATED PRECIPITATE OF COBALT OXALATE WITH A SECOND MEDIUM CONSISTING ESSENTIALLY OF ACETIC ACID CONTAINING ABOUT 3 TO 15 PERCENT WATER BY WEIGHT PROVIDED AT AN ELEVATED TEMPERATURE OF ABOUT 60 TO 140*C. AND CONTAINING CALCIUM IONS DISSOLVED THEREIN IN A QUANTITY AT LEAST EQUIVALENT STOICHIOMETRICALLY THE COBALT (II) IONS CONTAINED IN SAID COBALT OXALATE TO FORM CALCIUM OXALATE, (E) FORMING A SOLID PRECIPITATE OF CALCIUM OXALATE IN SAID SECOND ACETIC ACID MEDIUM WHILE SAID COBALT (II) IONS ARE SOLUBILIZED, AND (F) SEPARAING SAID SOLID PRECIPITATE OF CALCIUM OXALATE FROM SAID SECOND ACETIC ACID MEDIUM TO PRODUCE A FRESH SOLUTION OF CO(II) IONS DISSOLVED IN ACETIC ACID.