Abstract:
An improved process for the manufacture of cyclohexanone oxime by reacting cyclohexanone with an aqueous hydroxylammonium-ammonium sulfate solution at temperatures above the melting point of cyclohexanone oxime by the countercurrent process, the improvement consisting in that the reaction is carried out in the absence of solvents and neutralizing and/or buffer salts at pHs of up to 0.5 until equilibrium is reached, the oximes resulting during the reaction being separated from the aqueous phase and the aqueous phase being extracted with cyclohexanone and then subjected to steam distillation.
Abstract:
Continuous production of lactams by rearrangement of cycloalkanone oximes at from 210.degree. to 450.degree.C in contact with a supported catalyst in a fluidized bed wherein from 0.01 to 1 kg of steam is introduced above the fluidized bed for each kg of cycloalkanone oxime supplied. Lactams are starting materials for the production of synthetic polyamides suitable for fibers.
Abstract:
A process for producing lactam by Beckmann rearrangement of cycloalkanone oxime. A cycloalkanone oxime is contacted at an elevated temperature, with sulfate or phosphate of metal ions selected from manganese, ferrous, ferric, cobalt, nickel, zinc and cadmium in the presence of at least one mole of hydrogen chloride per mole of the cycloalkanone oxime. Lactam can be recovered from the reaction mixture without producing ammonium sulfate as a by-product.
Abstract:
1. IN A PROCESS FOR THE RECOVERY PURE E-CAPROLACTAM CONTAINING LESS THAN 5 MEQ. OF IONOGENIC SUBSTANCES PER KG. OF LACTAM, OBTAINED BY INTRAMOLECULAR CONVERSION OF CYCLOHEXANONE OXIME WITH THE AID OF AN ACID CATALYST FROM THE GROUP CONSISTING OF SULFURIC ACID, OLEUM AND SULPHUR TRIOXIDE, AND EXTRACTION OF THE REACTION MIXTURE AFTER DILUTION WITH WATER AND, OPTIONALLY AFTER PARTIAL NEUTRALIZATION OF THE SULPHURIC ACID, WITH A WATER-IMMISCIBLE ORGANIC SOLVENT FOR THE LACTAM, THE IMPROVEMENT COMPRISING NEUTRALIZING THE RESULTING SOLVENT OF LACTAM IN THE ORGANIC SOLVENT WITH AQUEOUS AMMONIA TO A PH OF AT LEAST 4.5 (MEASURED AT 20* C.), THEREBY FORMING AN EMULSION OF AN AQUEOUS 15-40% WT. AMMONIUM SULPHATE SOLUTION EMULSIFIED IN THE ORGANIC SOLVENT, WASHING THE EMULSION WITH A COUNTERFLOW OF DEMINERALIZED WATER IN A WEIGHT RATIO OF 4-20 PARTS THEREBY REESTRACTING THE LACTAM FROM THE ORGANIC SOLVENT TO PRODUCE AN ECAPROLACTAM SOLUTION WITH LESS THAN 5 MEQ. OF IONOGENIC SUBSTANCES PER KG. OF LACTAM, WHILE THE RESULTING AQUEOUS LACTAM SOLUTION IS EVAPORATED, OPTIONALLY AFTER HAVING BEEN FREED OF ORGANIC IONGENIC COMPOUNDS ON CATION AND ANION EXCHANGERS.
Abstract:
1. ABRASION-RESISTANT CATALYST CONTAINING BORIC ACID AND BORON NITRIDE SUITABLE FOR THE PREPARATION OF LACTAMS BY THE REARRANGEMENT OF CYCLIC KETOXIMES CONTAINING 5 TO 12 CARBON ATOMS IN THE RING IN THE GASEOUS PHASE AT A TEMPERATURE OF 200*C, TO 400:C., OBTAINED BY HEATING AT A TEMPERATURE OF 250* TO 900*C. (A) A MIXTURE OF BORIC ACID AND A SUPPORTING MATERIAL OF 1:4 TO 3:2, AND (B) -030% ACID: SUPPORTING MATERIAL OF 1:4 TO 3:2, AND (B) 1-30% BY WEIGHT BASED ON (A) OF A NITROGEN-CONTAINING COMPOUND WHICH FORMS BORON NITRIDE WITH BORIC ACID OR BORON TRIOXIDE SELECTED FROM THE GROUP CONSISTING OF HN4OH, (NH4)2CO3, NH4CL, UREA, GUANIDINE AND THIOUREA.
Abstract:
IMPROVEMENT IN THE PROCESS FOR THE CATALYTIC REARRANGEMENT OF CYCLIC KETOXIMES TO LACTAMS USING A BORON OXIDE CATALYST, THE CATALYST BEING REGENERATED BY ADDING AN ORTHOBORIC ACID ALKYLESTER WHILE BEING IN THE FLUIDISED STATE AT TEMPERATURES OF FROM 200-800*C.
Abstract:
THE INVENTION RELATES TO A PROCESS FOR THE PRODUCTION OF LACTAMS BY CATALYTICAL REARRANGEMENT OF KETOXIMES IN THE GASEOUS PHASE, USING AS A CATALYST SYSTEM A MIXTURE OF BORON TRIOXIDE OR BORIC ACID, HIGHLY DISPERSED CARBON, AND ONE OR MORE ADDITIONAL INORGANIC SUPPORTING MATERIAL, SAID HIGHLY DISPERSED CARBON HAVING A PARTICLE SIZE OF LESS THAN 0.1MM. IN DIAMETER.
Abstract:
IMPROVEMENT IN THE PROCESS FOR THE CATALYTIC REARRANGEMENT OF CYCLIC KETOXIMES TO LACTAMS USING A BORON OXIDE CATALYST, THE LOSS OF BORON OXIDE BEING AVOIDED BY SEPARATING FROM THE REACTION PRODUCTS A PRIMARY CONDENSATE AT TEMPERATURES OF FROM 120 TO 220*C., CONTAINING BORIC ACID AND ISLOATE THIS BORIC ACID FROM THE PRIMARY CONDENSATION PRODUCT BY ESTERIFICATION WITH A MONODYDRIC ALIPHATIC ALCOHOL TO YIELD AN ORTHOBORIC ACID TRIALKYLESTER WHICH IS HYDROLYZED TO PURE BORIC ACID.
Abstract:
A PROCESS FOR THE CONTINUOUS PRODUCTION OF LACTAMS WHICH ARE STARTING MATERIALS FOR NYLON-TYPE POLYAMIDES, FROM CYCLIC KETOXIMES, USING MINERAL ACIDS AS A CATALYST, CYCLING OXIME AND ACID BY WAY OF NOZZLES FROM CONTINUOUS MIXERS IN LIEU OF USING AGITATOR VESSELS. THE NOZZLE DELIVERY SPEED OF THE OXIME AND OF THE ACID IS AT LEAST TWICE THE FLOW VELOCITY OF THE CYCLE AND THE VOLUME PROPORTIONS OF THE PRODUCT PUMPED PER HOUR TO OXIME INTRODUCED IS 50:1 TO 150:1.