公开(公告)号：US4873325A

公开(公告)日：1989-10-10

申请号：US878215

申请日：1986-06-25

Applicant: Kurt D. Olson

Inventor： Kurt D. Olson

IPC: B01J29/04 ,  B01J29/84 ,  B01J29/85 ,  B01J29/86 ,  C07B31/00 ,  C07B43/06 ,  C07C67/00 ,  C07D201/04

CPC classification number: C07D201/04 ,  B01J29/84 ,  B01J29/86

Abstract: Oximes can be converted to the corresponding amides by contacting the oximes with a non-zeolitic molecular sieve, which has in its calcined form an adsorption of isobutane of at least about 2 percent by weight of the non-zeolitic molecular sieve at a partial pressure of 500 torr and a temperature of 20.degree. C. The process is especially useful for the conversion of cyclohexanone oxime to caprolactam. The non-zeolitic molecular sieves can achieve improved conversion rates and selectivities as compared with conventional zeolite catalysts for the reaction.

Abstract translation: 肟可以通过使肟与非沸石分子筛接触而转化为相应的酰胺，该非沸石分子筛在其煅烧形式下吸附至少约2重量％的非沸石分子筛的异丁烷，分压 500托，温度为20℃。该方法特别适用于将环己酮肟转化为己内酰胺。 与用于反应的常规沸石催化剂相比，非沸石分子筛可以实现改进的转化率和选择性。

公开(公告)号：US4804754A

公开(公告)日：1989-02-14

申请号：US130949

申请日：1987-12-10

Applicant: Emile De Decker ,  Jozef Oostvogels ,  Gerard van Wauwe ,  Gerald Neubauer

Inventor： Emile De Decker ,  Jozef Oostvogels ,  Gerard van Wauwe ,  Gerald Neubauer

IPC: C07D201/04 ,  C07D201/16

CPC classification number: C07D201/04

Abstract: Caprolactam is prepared in a process comprising(a) a Beckmann rearrangement of cyclohexanone oxime with oleum at from 70.degree. to 130.degree. C. in one or more rearrangement stages, and(b) aftertreatment of the reaction mixture obtained from the rearrangement stage in a delay zone at from 70.degree. to 110.degree. C. for from 10 to 600 minutes.

Abstract translation: 在一个方法中制备己内酰胺，该方法包括（a）在一个或多个重排阶段中，环己酮肟与发烟硫酸在发酵油中的贝克曼重排在70〜130℃，（b）后处理从重排阶段获得的反应混合物 延迟区为70〜110℃，时间为10〜600分钟。

公开(公告)号：US4248782A

公开(公告)日：1981-02-03

申请号：US78031

申请日：1979-09-24

Applicant: Hugo Fuchs ,  Uwe Brand ,  Peter Horn

Inventor： Hugo Fuchs ,  Uwe Brand ,  Peter Horn

IPC: C07D201/04

CPC classification number: C07D201/04 ,  Y02P20/52

Abstract: In a process for the preparation of .epsilon.-caprolactam by catalytic rearrangement of cyclohexanone-oxime in the gas phase at from 230.degree. to 450.degree. C. over a supported catalyst, containing boron trioxide, in a fluidized bed, wherein the catalyst is removed from the fluidized bed at the rate at which it becomes spent and is treated, in a fluidized state, with gases containing molecular oxygen at from 600.degree. to 900.degree. C., after which boron trioxide or boric acid is added to the fluidized catalyst, at from 300.degree. to 900.degree. C., before the catalyst is returned to the fluidized bed, the improvement that boron trioxide or boric acid of particle size from 0.05 to 1.5 mm is fed to the fluidized catalyst at one or more points.

Abstract translation: 在通过在230℃至450℃的气相中催化重排环己酮 - 肟在含有三氧化硼的载体催化剂的流化床中制备ε-己内酰胺的方法，其中将催化剂从 流化床以其流失的速率以流化状态处理含有分子氧的气体在600-900℃，之后将三氧化硼或硼酸加入到流化催化剂中，在 在催化剂返回到流化床之前，从300℃升至900℃，改善将粒径为0.05-1.5mm的三氧化硼或硼酸以一个或多个点进料到流化催化剂中。

公开(公告)号：US4211700A

公开(公告)日：1980-07-08

申请号：US12495

申请日：1979-02-15

Applicant: Jean-Claude Michel ,  Philippe Potin

Inventor： Jean-Claude Michel ,  Philippe Potin

IPC: C07D201/10 ,  C07D201/04

CPC classification number: C07D201/04

Abstract: The invention relates to a process for the preparation of lactames according to the so-called "Beckmann rearrangement" which consists in isomerizing oximes in a sulfuric solution, the weight ratio percentage of sulfuric acid to the combined amount of sulfuric acid and water being raised to a value above that of the sulfuric solution feed.

Abstract translation: 本发明涉及一种根据所谓的“贝克曼重排”制备内酰胺的方法，该方法包括在硫酸溶液中异构化肟，硫酸与硫酸和水的混合量的比例百分比提高至 值高于硫酸溶液进料的值。

公开(公告)号：US4141896A

公开(公告)日：1979-02-27

申请号：US832008

申请日：1977-09-09

Applicant: Otto Immel ,  Andre DE Jager ,  Bernd-Ulrich Kaiser ,  Hans-Helmut Schwarz ,  Klaus Starke

Inventor： Otto Immel ,  Andre DE Jager ,  Bernd-Ulrich Kaiser ,  Hans-Helmut Schwarz ,  Klaus Starke

IPC: C07D201/02 ,  C07D201/04

CPC classification number: C07D201/04

Abstract: A process for the production of .epsilon.-caprolactum from cyclohexanone oxime by rearrangement in the gaseous phase on a fluid-bed catalyst containing boron oxide, wherein residues from the distillation of cyclohexanone oxime are introduced into the reaction in liquid form, and wherein from 5 to 500 times their quantity of cyclohexanone oxime in vapor form and at least 50 times their quantity of inert gas are present during the reaction.

Abstract translation: 一种通过在含有氧化硼的流化床催化剂上在气相中重新排列从环己酮肟生产ε-己内酰胺的方法，其中将来自环己酮肟蒸馏的残余物以液体形式引入反应中，其中从5至 蒸气形式的环己酮肟的量为其500倍，并且在反应期间存在至少50倍量的惰性气体。

公开(公告)号：US4031139A

公开(公告)日：1977-06-21

申请号：US652421

申请日：1976-01-26

Applicant: Guenther Rapp ,  Hugo Fuchs ,  Erwin Thomas

Inventor： Guenther Rapp ,  Hugo Fuchs ,  Erwin Thomas

IPC: C07D223/08 ,  C07C67/00 ,  C07C239/00 ,  C07C251/46 ,  C07D201/04 ,  C07D223/10 ,  C07C131/04

CPC classification number: C07D201/04

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 translation: 通过逆流法在环己酮肟的熔点以上的温度下使环己酮与羟基铵 - 硫酸铵水溶液反应制备环己酮肟的改进方法，其改进在于反应在不存在溶剂的情况下进行， 中和和/或缓冲盐的pH值高达0.5，直到达到平衡，反应中产生的肟与水相分离，水相用环己酮萃取，然后进行蒸汽蒸馏。

公开(公告)号：US3954736A

公开(公告)日：1976-05-04

申请号：US84546

申请日：1970-10-27

Applicant: Norbert Petri

Inventor： Norbert Petri

IPC: B01J8/24 ,  C07B61/00 ,  C07D201/04

CPC classification number: C07D201/04

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 translation: 通过在210℃至450℃下重新排列与负载型催化剂接触的流化床中连续生产内酰胺，其中在流化床上将0.01至1kg蒸汽引入每kg供应的环烷酮肟。 内酰胺是用于生产适用于纤维的合成聚酰胺的起始原料。

公开(公告)号：US3904608A

公开(公告)日：1975-09-09

申请号：US39471473

申请日：1973-09-06

Applicant: TORAY INDUSTRIES

Inventor： TAKAYANAGI KAZUO ,  SONODA TAKESHI

IPC: C07D223/12 ,  B01J27/00 ,  C07B61/00 ,  C07D201/04

CPC classification number: C07D201/04 ,  Y02P20/52

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.

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

IPC: C07D201/04 ,  C07D201/16 ,  C07D41/06

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.

公开(公告)号：US3849335A

公开(公告)日：1974-11-19

申请号：US13149671

申请日：1971-04-05

Applicant: BAYER AG

Inventor： IMMEL O ,  SCHWARZ H

IPC: B01J27/24 ,  B01J31/12 ,  C07D201/04 ,  C07D41/04

CPC classification number: C07D201/04 ,  B01J27/24

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.