Processing polycaprolactam extraction liquors
    71.
    发明授权
    Processing polycaprolactam extraction liquors 失效
    加工聚己内酰胺提取液

    公开(公告)号:US3992372A

    公开(公告)日:1976-11-16

    申请号:US560313

    申请日:1975-03-20

    CPC classification number: C08G69/46

    Abstract: A process for processing polycaprolactam extraction liquors by evaporation of water and distillation of the residue in which the evaporation of water is carried out in a plurality of stages and the evaporation energy for the removal of the bulk of the water is taken from the heat liberated in the rearrangement of cyclohexanone oxime to caprolactam in oleum or sulfuric acid by using the extraction water for cooling the rearrangement mixture and utilizing the heat absorbed by the extraction water for the concentration of this extraction water by evaporation of water.

    Abstract translation: 通过蒸发水处理聚己内酰胺提取液的方法,并且蒸馏残留物,其中水的蒸发在多个阶段中进行,并且用于除去大部分水的蒸发能源取自在 通过使用提取水冷却重排混合物并利用由萃取水吸收的热量,通过蒸发水将该萃取水浓缩,将环己酮肟重排为己内酰胺在发烟硫酸或硫酸中。

    Process for the purification of caprolactam
    72.
    发明授权
    Process for the purification of caprolactam 失效
    己内酰胺纯化方法

    公开(公告)号:US3966712A

    公开(公告)日:1976-06-29

    申请号:US519687

    申请日:1974-10-31

    CPC classification number: C07D201/16

    Abstract: Object of the invention is a process for the purification of a caprolactam obtained by catalytic rearrangement of cyclohexanone oxime in the gaseous phase comprising crystallization said caprolactam which main impurity consists of cyclohexanone oxime from dimethylformamide, dimethylacetamide, methyl formate, ethyl formate, methyl acetate, tetrahydrofuran, 1,3 dioxane, 1,4 dioxane, propanol, butanol or amyl alcohol or from a mixture of these solvents, followed by distillation.

    Abstract translation: 本发明的目的是通过在气相中催化重排环己酮肟而获得的己内酰胺的纯化方法,包括结晶所述己内酰胺,其主要杂质由二甲基甲酰胺,二甲基乙酰胺,甲酸甲酯,甲酸乙酯,乙酸甲酯,四氢呋喃 ,1,3-二恶烷,1,4-二恶烷,丙醇,丁醇或戊醇,或这些溶剂的混合物,然后进行蒸馏。

    Process for the neutralization of acid solutions of caprolactam
    73.
    发明授权
    Process for the neutralization of acid solutions of caprolactam 失效
    过氧化氢中和酸解决方案的中和方法

    公开(公告)号:US3937789A

    公开(公告)日:1976-02-10

    申请号:US425171

    申请日:1973-12-14

    CPC classification number: C07D201/16 C01C1/242

    Abstract: A process is disclosed in which the heat generated, during neutralization,y ammonium sulfate of a solution of .xi.-caprolactam in sulfuric acid, is used to effect evaporation of water present, and the temperature is kept at about 40.degree.C to 50.degree.C, under subatmospheric pressure, so that substantial hydrolysis of the caprolactam is avoided while a substantial portion of the water present in the neutralization mixture is evaporated at the subatmospheric pressure, and the ammonium sulfate is crystallized substantially free from entrained caprolactam. The caprolactam is then separated from the aqueous phase.

    Process for the recovery of pure epsilon-caprolactam
    74.
    发明授权
    Process for the recovery of pure epsilon-caprolactam 失效
    恢复纯EPSILON-CAPROLACTAM的方法

    公开(公告)号:US3850910A

    公开(公告)日:1974-11-26

    申请号:US30172672

    申请日:1972-10-30

    Applicant: STAMICARBON

    Inventor: GOETTSCH R VOS H

    CPC classification number: C07D201/04 C07D201/16

    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.

    Refining process and refining system of caprolactam

    公开(公告)号:US11459302B2

    公开(公告)日:2022-10-04

    申请号:US17208073

    申请日:2021-03-22

    Abstract: A refining process includes steps of subjecting crude caprolactam to a first evaporative crystallization and a first solid-liquid separation to obtain a first caprolactam crystal and a first crystallization mother liquor; washing the first caprolactam crystal to obtain a second caprolactam crystal; optionally concentrating the first crystallization mother liquor to perform a second evaporative crystallization and a second solid-liquid separation to obtain a third caprolactam crystal and a second crystallization mother liquor; subjecting the third caprolactam crystal to a second washing to obtain a fourth caprolactam; optionally concentrating the second crystallization mother liquor to perform thermostatic crystallization, performing separation to obtain a fifth caprolactam crystal and a third crystallization mother liquor; washing the fifth caprolactam crystal to obtain a sixth caprolactam crystal; and subjecting the second caprolactam crystal to a hydrogenation reaction.

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