Abstract:
In a process for the preparation of lactam from cycloalkanone comprising reacting said alkanone with hydroxylamine sulfate to form the corresponding cycloalkanone oxime followed by Beckman rearrangement to yield said lactam and neutralization of the sulfuric acid formed by ammonia whereby ammonium sulfate is formed as a byproduct, the improvement which comprises reacting said ammonium sulfate with an alkaline-earth metal oxide or hydroxide to form an alkaline earth metal sulfate and ammonia, heating said alkaline-earth metal sulfate to decompose it into said alkaline-earth metal oxide and sulfur dioxide and/or sulfur trioxide, converting said sulfur dioxide and/or sulfur trioxide into sulfuric acid, whereby said sulfuric acid and said ammonia are capable of reuse in said process.
Abstract:
Epsilon -CAPROLACTAM MATERIAL SUCH AS A MONOMER, OLIGOMERS AND POLYMERS OF Epsilon -CAPROLACTAM AND MIXTURES OF THESE COMPOUNDS ARE PURIFIED FROM IMPURITY COMPOUNDS SUCH AS PHOSPHORIC ACID AND IONIZED METAL COMPOUNDS CONTAINED THEREIN BY BRINGING THE Epsilon -CAPROLACTAM MATERIAL INTO CONTACT WITH AN AQUEOUS SOLUTION CONTAINING 15 TO 75 PERCENT BY WEIGHT OF AT LEAST ONE ALKALI METAL PHOSPHATE TO EXTRACT THE IMPURITY COMPOUND FROM THE Epsilon -CAPROLACTAM MATERIAL INTO THE PHOSPHATE AQUEOUS SOLUTION AND, THEREAFTER, SEPARATING THE Epsilon -CAPROLACTAM MATERIAL FROM THE PHOSPHATE AQUEOUS SOLUTION BY WAY OF SETTLING OR CENTRIFUGING THE MIXTURE.
Abstract:
Caprolactam is recovered from a mixture which contains caprolactam and oligomers of the same by distillation at temperatures above the melting point of the oligomers or mixture thereof contained in the residue at atmospheric or slightly increased pressure. The process is of importance for removing residues of caprolactam oligomer residues and thus for effluent pollution control.
Abstract:
A continuous process for the purification of caprolactam characterized in that raw caprolactam is subjected to a solvent distillation followed by a distillation under reduced pressure in the presence of sodium hydroxide and then to a melt crystallization, in which: A. The residue from the alkaline distillation is taken up in water, the aqueous solution extracted with benzene or toluene and the lactam solution fed to the main product stream through the solvent distillation; B. The residue from the melt crystallization is extracted in the crystalline state with an aliphatic or cycloaliphatic hydrocarbon with 5-10 carbon atoms and the purified residue is fed back into the alkaline distillation of the main produce stream; and C. The aliphatic or cycloaliphatic hydrocarbon is regenerated and used again for the extraction of the residue from the meltcrystallization.
Abstract:
A PROCESS CHARACTERIZED IN THAT RAW CAPROLACTAM IS SUBJECTED, IN EITHER SEQUENCE, TO A CRYSTAL EXTRACTION WITH AN ALIPHATIC OR CYCLOALIPHATIC HYDROCARBON HAVING 5-10 CARBON ATOMS AND TO DISTILLATION UNDER REDUCED PRESSURE.
Abstract:
A PROCESS FOR THE SEPARATION OF LOWER BOILING POINT LIQUIDS FROM THOSE OF A HIGH BOILING POINT, AND APPARATUS THEREFOR IS DISCLOSED. THE LIQUID MIXTURE IS SUPPLIED TO THE BASE OF THE EXTRACTOR AND PASSED UPWARDS UNDER CONTROLLED TEMPERATURE AND REDUCED PRESSURE IN THE VAPOR STATE THROUGH SEVERAL TUBES, WHOSE LENGTH IS FROM 15 TO 35 TIMES THEIR DIAMETER; THE VAPOR LEAVES THE TUBES AT A
VELOCITY APPROACHING THE VELOCITY OF SOUND IN THE VAPOR, AND IS SUBSEQUENTLY CONDENSED. THE LOWER BOILING LIQUID THUS RECOVERED IS OF HIGH PURITY, OFTEN REPRESENTING UP TO 90% OF THE TOTAL LOWER BOILING FRACTION OF THE MIXTURE ENTERING THE EVAPORATOR.
Abstract:
Laurolactam is purified by crystallization from solution in a solvent mixture of acetonitrile and water. The water content of the solvent mixture does not exceed 45 percent. Laurolactams thus purified are useful in the preparation of polyamides.
Abstract:
A process for the recovery of p-dichlorobenzene and Nmethylpyrrolidone from the reactor effluent from the production of polyphenylene sulfide from which the polyphenylene sulfide has been separated involving a steam distillation step to recover the p-dichlorobenzene and a fractionation step to recover the Nmethylpyrrodone.
Abstract:
RECOVERING ACIDS AND ORGANIC BASES FROM THEIR SALTS BY HEATING THE SALT TO ITS DISSOCIATION TEMPERATURE AND REMOVING THEREFROM THE ACID OR BASE WHEREIN THE SALT DISSOCIATES AT A TEMPERATURE LOWER THAN THE DECOMPOSITION TEMPERATURES OF THE ACID AND BASE; THE ACID AND BASE HAVE DIFFERENT VOLATILITIES AND THE SALT HAS A SUBLIMATION TEMPERATURE HIGHER THAN THE DISSOCIATION TMPERATURE THEREOF.
Abstract:
1,105,489. Concentrating liquids by freezing. PHILLIPS PETROLEUM CO. 2 Aug., 1965 [14 Aug., 1964], No. 33015/65. Heading F4H. In a process for separating the components of a liquid mixture by freezing, the crystal/ mother-liquor slurry from a freezer 2 is passed to a separator 16 from which the motherliquor is withdrawn at 9, the crystals are passed to a mixing vessel 18 where they are re-slurried with un-processed liquid from line 13, the slurry is passed to a purification column 20, and the mother liquor is withdrawn from an intermediate filter section 24 of the column and recycled through line 17 to form part or all of the liquid supply 1 for the freezer. The column further includes a reflux portion 30 and a heater 32 for melting the crystals, the melt being withdrawn through line 23 to which a pulsating pressure is applied by means 36. The freezer 2 is of the jacketed type including a scraper 8 but may be replaced by a direct contact heat exchanger. Liquids which may be treated in the process are sea-water, caprolactam, hydrocarbon mixtures such as para and meta-xylene and combinations of benzene n-heptane, carbon tetrachloride, ethyl alcohol, cyclohexane, methyl cyclohexane, toluene, chloroform, acetone and ethyl benzene, and food products such as grape, orange, lemon, pineapple, apple and tomato juices, vegetable juices, milk, beer, wine, coffee and tea. A quantitative example of the process as applied to the concentration of beer is given.