公开(公告)号：US20030105322A1

公开(公告)日：2003-06-05

申请号：US10258941

申请日：2002-10-29

Inventor： Peter Bassler ,  Dieter Baumann ,  Rolf-Hartmuth Fischer ,  Eberhard Fuchs ,  Johann-Peter Melder ,  Frank Ohlbach

IPC: C07D201/02

CPC classification number: C07D201/08

Abstract: A process for the preparation of caprolactam is provided, wherein a) a mixture (I) containing 6-aminocapronitrile and water is reacted in the gas phase, in the presence of a catalyst, to give a mixture (II) containing caprolactam, ammonia, water, high-boiling components and low-boiling components, b) ammonia is then removed from the mixture (II) to give a mixture (III) containing caprolactam, water, high-boiling components and low-boiling components, c) water is then removed from the mixture (III) to give a mixture (IV) containing caprolactam, high-boiling components and low-boiling components, and d) a solid (V) containing caprolactam is then obtained from the mixture (IV) by crystallization, the proportion by weight of caprolactam in the solid (V) being greater than in the mixture (IV).

Abstract translation: 提供了制备己内酰胺的方法，其中a）含有6-氨基己腈和水的混合物（I）在气相中在催化剂存在下反应，得到含有己内酰胺，氨， 水，高沸点组分和低沸点组分，b）然后从混合物（II）中除去氨，得到含有己内酰胺，水，高沸点组分和低沸点组分的混合物（III），c）水是 然后从混合物（III）中取出，得到含己内酰胺，高沸点成分和低沸点组分的混合物（Ⅳ），然后通过结晶从混合物（Ⅳ）中获得含有己内酰胺的固体（Ⅴ） 固体（V）中己内酰胺的重量比例大于混合物（IV）中的比例。

公开(公告)号：US20030065169A1

公开(公告)日：2003-04-03

申请号：US10210878

申请日：2002-08-02

Applicant: DSM N.V.

Inventor： Frank P.W. Agterberg ,  Rudolf P.M. Guit ,  Matthias R.J. Offermanns

IPC: C07D21/08 ,  C08G069/08 ,  C08G073/10

CPC classification number: C07D201/12 ,  C07D201/08

Abstract: A process for the preparation of null-caprolactam starting from 6-aminocaproic acid, 6-aminocaproamide, 6-aminocaproic ester, 6-aminocapronitrile, oligomers or polymers of these compounds or mixtures comprising at least two of these compounds, which process is performed in the presence of N-(5-carboxypentyl)-null-caprolactam and/or derivative thereof in an amount of less than 50 wt. % and more than 0.1 wt. % (based on the total reaction mixture).

Abstract translation: 从6-氨基己酸，6-氨基己酰胺，6-氨基己酸酯，6-氨基己腈，这些化合物的低聚物或聚合物或包含这些化合物中的至少两种的混合物制备ε-己内酰胺的方法，该方法在 N-（5-羧戊基） - 己内酰胺和/或其衍生物的存在量小于50wt。 ％和大于0.1wt。 ％（基于总反应混合物）。

公开(公告)号：US06452002B2

公开(公告)日：2002-09-17

申请号：US09795706

申请日：2001-03-01

Applicant: Robert Pestman ,  Lambertus H. W. M. Van Lieshout

Inventor： Robert Pestman ,  Lambertus H. W. M. Van Lieshout

IPC: C07D20108

CPC classification number: C07C227/08 ,  C07C231/14 ,  C07D201/08 ,  Y02P20/52

Abstract: Process for preparing an aqueous mixture of &egr;-caprolactam and 6-aminocaproic acid and/or 6-aminocaproamide which involves, as the reductive amination step, contacting 5-formylvaleric acid and/or an alkyl 5-formylvalerate in water as solvent with hydrogen and an excess of ammonia in the presence of a ruthenium on carrier, as a catalyst, wherein the carrier is titanium oxide, zirconium oxide, graphite or carbon and the catalyst also contains at least one of the metals of group 8-11, or a compound of these metals. The aqueous mixture can be used to prepare &egr;-caprolactam.

Abstract translation: 制备ε-己内酰胺和6-氨基己酸和/或6-氨基己酰胺的水性混合物的方法，其涉及作为还原胺化步骤，将5-甲酰基戊酸和/或作为溶剂的5-甲酰基戊酸烷基酯与氢气和/ 在载体上的钌存在下的过量氨，作为催化剂，其中载体是氧化钛，氧化锆，石墨或碳，并且催化剂还含有至少一种第8-11族的金属或化合物 的这些金属。 含水混合物可用于制备ε-己内酰胺。

公开(公告)号：US20020120154A1

公开(公告)日：2002-08-29

申请号：US10017222

申请日：2001-12-14

Applicant: Dairen Chemical Corporation

Inventor： Shien-Chang Chen ,  Fu-Shen Lin ,  Liang-An Hsu ,  Cheng-Lin Tsai ,  Joe-Min Lin

IPC: C07D27/26 ,  C07D211/40

CPC classification number: C07D207/267 ,  C07D201/08

Abstract: The present invention is related to a method for preparing lactam represented by the following formula: 1 wherein R is C2-10 alkylene which may be optionally substituted with C1-6 alkyl or phenyl; Rnull is a hydrogen atom, C1-6, alkyl, C1-6 hydroxyalkyl or phenyl. The method for preparing lactam comprises an amination reaction using crystalline aluminosilicate zeolites as catalysts under the condition of gas phase in the presence of (a) lactone, (b) amine and/or ammonia and (c) water.

Abstract translation: 本发明涉及一种由下式表示的制备内酰胺的方法：其中R是可被C1-6烷基或苯基任意取代的C 2-10亚烷基; R'是氢原子，C 1-6，烷基，C 1-6羟基烷基或苯基。 制备内酰胺的方法包括在（a）内酯，（b）胺和/或氨和（c）水的存在下，在气相条件下使用结晶硅铝酸盐沸石作为催化剂的胺化反应。

公开(公告)号：US06372939B1

公开(公告)日：2002-04-16

申请号：US09713143

申请日：2000-11-16

Applicant: Emilio E. Bunel ,  Theodore A. Koch ,  Ronnie Ozer ,  Sourav K. Sengupta

Inventor： Emilio E. Bunel ,  Theodore A. Koch ,  Ronnie Ozer ,  Sourav K. Sengupta

IPC: C07C20500

CPC classification number: C07D201/08 ,  C07C227/06 ,  C07C253/30 ,  C07C229/08 ,  C07C255/07 ,  C07C255/17 ,  C07C255/19

Abstract: A process for making 6-aminocaproic acid by hydroformylating 3-pentenenitrile to produce 3-, 4-, and 5-formylvaleronitrile (FVN mixture), oxidizing the FVN mixture to produce 3-, 4-, and 5-cyanovaleric acid; hydrogenating the resulting product to produce 6-aminocaproic acid, 5-amino-4-methylvaleric acid, and 4-amino-3-ethylbutyric acid; and isolating 6-aminocaproic acid from the reaction product. The resulting 6-aminocaproic acid can be cyclized to produce caprolactam.

Abstract translation: 通过加氢甲酰化3-戊烯腈生产3-，4-和5-甲酰基戊腈（FVN混合物）制备6-氨基己酸的方法，氧化FVN混合物以产生3-，4-和5-氰基戊酸; 氢化所得产物以产生6-氨基己酸，5-氨基-4-甲基戊酸和4-氨基-3-乙基丁酸; 并从反应产物中分离出6-氨基己酸。 所得6-氨基己酸可以环化以制备己内酰胺。

公开(公告)号：US06333412B1

公开(公告)日：2001-12-25

申请号：US09635717

申请日：2000-08-09

Applicant: Rudolf P. M. Guit ,  Samuel L. Lane

Inventor： Rudolf P. M. Guit ,  Samuel L. Lane

IPC: C07D20108

CPC classification number: C07D201/08

Abstract: Process to prepare &egr;-caprolactam starting from a starting mixture containing a 6-aminocaproate ester, in which in a first step (1) the 6-aminocaproate ester is converted into 6-aminocaproic acid and 6-aminocaproamide by reaction with water in the presence of ammonia at a temperature of between 50 and 250° C., with a separate or simultaneous removal of alcohol(s), and in a subsequent step (2) the 6-aminocaproic acid and 6-aminocaproamide are cyclizised at an elevated temperature, wherein in step (1) the 6-aminocaproate ester is converted into 6-aminocaproic acid and 6-aminocaproamide in the presence of an amount higher than 2 wt. % and less than or equal to 25 wt. % NH3 (relative to the total amount of organic compounds, water and ammonia present in step (1)).

Abstract translation: 从含有6-氨基己酸酯的起始混合物制备ε-己内酰胺的方法，其中在第一步（1）中，6-氨基己酸酯在存在下与水反应转化为6-氨基己酸和6-氨基己酰胺 在50至250℃的温度下，分离或同时除去醇，并且在随后的步骤（2）中，6-氨基己酸和6-氨基己酰胺在升高的温度下环化， 其中在步骤（1）中，将6-氨基己酸酯在高于2重量％的量存在下转化成6-氨基己酸和6-氨基己酰胺。 ％且小于或等于25wt。 ％NH 3（相对于步骤（1）中存在的有机化合物，水和氨的总量）。

公开(公告)号：US06323341B1

公开(公告)日：2001-11-27

申请号：US09665592

申请日：2000-09-19

Applicant: Frank P. W. Agterberg ,  Rudolf P. M. Guit ,  Nicolaas F. Haasen

Inventor： Frank P. W. Agterberg ,  Rudolf P. M. Guit ,  Nicolaas F. Haasen

IPC: C07D20116

CPC classification number: C07D201/08 ,  C07D201/16

Abstract: The invention relates to a process for the purification of crude &egr;-caprolactam, wherein crude &egr;-caprolactam prepared by cyclization of alkyl 6-aminocaproate, 6-aminocapronitrile, 6-aminocaproic acid, 6-aminocaproic amide and/or oligomers thereof, is subjected to a crystallization process.

Abstract translation: 本发明涉及纯化ε-己内酰胺的方法，其中将通过6-氨基己酸烷基酯，6-氨基己腈，6-氨基己酸，6-氨基己酰胺和/或其低聚物的环化制备的粗ε-己内酰胺进行 结晶过程。

公开(公告)号：US06300496B1

公开(公告)日：2001-10-09

申请号：US09413572

申请日：1999-10-06

Applicant: Kurt Damar Olson ,  Thomas Carl Eisenschmid ,  David Robert Bryant ,  Arthur Roy Doumaux, Jr.

Inventor： Kurt Damar Olson ,  Thomas Carl Eisenschmid ,  David Robert Bryant ,  Arthur Roy Doumaux, Jr.

IPC: C07D20108

CPC classification number: C07D201/08 ,  Y02P20/582

Abstract: This invention relates in part to processes for producing one or more substituted or unsubstituted epsilon caprolactams, e.g., epsilon caprolactam, which comprise (a) converting one or more substituted or unsubstituted hydroxyaldehydes, e.g., 6-hydroxyhexanal, optionally in the presence of a catalyst or a catalyst and promoter, to one or more substituted or unsubstituted hydroxyamides, e.g. 6-hydroxycaproamide, and/or one or more substituted or unsubstituted epsilon caprolactam precursors, e.g., 6-aminocaproamide, epsilon caprolactone, epsilon caprolactone oligomers and esters of 6-hydroxycaproic acid and mixtures thereof, and (b) converting said one or more substituted or unsubstituted hydroxyamides and/or said one or more substituted or unsubstituted epsilon caprolactam precursors, optionally in the presence of a catalyst or a catalyst and promoter, to said one or more substituted or unsubstituted epsilon caprolactams; wherein the amount of byproducts resulting from reduction and/or reductive amination of said one or more substituted or unsubstituted hydroxyaldehydes, e.g., 1,6-hexanediol, aminohexanol, and the like, is no greater than about 10 weight percent, preferably no greater than about 5 weight percent, and more preferably no greater than about 1 weight percent, of the total of said one or more substituted or unsubstituted hydroxyamides and/or one or more substituted or unsubstituted epsilon caprolactam precursors. This invention also relates in part to reaction mixtures containing one or more substituted or unsubstituted epsilon caprolactams as principal product(s) of reaction.

Abstract translation: 本发明部分地涉及用于制备一种或多种取代或未取代的ε-己内酰胺（例如ε-己内酰胺）的方法，其包括（a）任选在催化剂存在下，将一种或多种取代或未取代的羟基醛例如6-羟基己醛转化 或催化剂和促进剂，与一种或多种取代或未取代的羟基酰胺，例如， 6-羟基己酰胺和/或一种或多种取代或未取代的ε-己内酰胺前体，例如6-氨基己酰胺，ε-己内酯，ε-己内酯低聚物和6-羟基己酸的酯及其混合物，和（b）将所述一种或多种取代的 或所述一种或多种取代或未取代的ε-己内酰胺前体，任选在催化剂或催化剂和促进剂存在下，与所述一种或多种取代或未取代的ε己内酰胺反应; 其中所述一种或多种取代或未取代的羟基醛（例如1,6-己二醇，氨基己醇等）的还原和/或还原胺化产生的副产物的量不大于约10重量％，优选不大于 所述一个或多个取代或未取代的羟基酰胺和/或一个或多个取代或未取代的ε-己内酰胺前体的总量的约5重量％，更优选不大于约1重量％。 本发明还部分涉及含有一种或多种取代或未取代的ε-己内酰胺作为主要反应产物的反应混合物。

公开(公告)号：US06262259B1

公开(公告)日：2001-07-17

申请号：US08875451

申请日：1999-10-28

Applicant: Marie-Christine Cotting ,  Laurent Gilbert ,  Nathalie Laurain ,  Christophe Nedez

Inventor： Marie-Christine Cotting ,  Laurent Gilbert ,  Nathalie Laurain ,  Christophe Nedez

IPC: C07D20108

CPC classification number: C07D201/08 ,  Y02P20/52 ,  Y02P20/582 ,  Y02P20/584

Abstract: The present invention includes a process for the preparation of a lactam by vapor phase reaction of an aliphatic aminonitrile with water in the presence of a solid catalyst, wherein the catalyst is an alumina having a specific surface, measured by the BET method, greater than or equal to 10 m2/g. The alumina catalyst is further characterized by either: (a) a specific surface less than or equal to 280 m2/g, and a volume of pores with a diameter greater than 500 Å which is greater than or equal to 10 ml/100 g; or (b) a specific surface greater than or equal to 50 m2/g and less than or equal to 280 m2/g, and a volume of pores with a diameter greater than 70 Å which is greater than or equal to 30 m2/g.

Abstract translation: 本发明包括在固体催化剂存在下通过脂族氨基腈与水的气相反应制备内酰胺的方法，其中催化剂是通过BET法测量的比表面积的氧化铝，大于或等于 等于10 m2 / g。 氧化铝催化剂的特征还在于：（a）小于或等于280m 2 / g的比表面积，以及直径大于500埃的孔体积大于或等于10ml / 100g; 或（b）大于或等于50m 2 / g且小于或等于280m 2 / g的比表面积，以及直径大于70埃的孔体积大于或等于30m 2 / g 。

公开(公告)号：US6037477A

公开(公告)日：2000-03-14

申请号：US74604

申请日：1998-05-08

Applicant: Yasutaka Ishii ,  Tatsuya Nakano

Inventor： Yasutaka Ishii ,  Tatsuya Nakano

IPC: C07D307/89 ,  B01J31/02 ,  B01J31/22 ,  C07B61/00 ,  C07C51/23 ,  C07C51/31 ,  C07C51/54 ,  C07C55/12 ,  C07C67/39 ,  C07C69/24 ,  C07C69/78 ,  C07D201/08 ,  C07D309/30 ,  C07D311/76 ,  C07D311/86 ,  C07D313/04 ,  C07D315/00 ,  C07D207/404 ,  C07D207/444 ,  C07D207/448 ,  C07D487/06

CPC classification number: C07D315/00 ,  B01J31/006 ,  B01J31/0247 ,  C07C51/23 ,  C07C51/54 ,  C07C67/39 ,  C07D201/08 ,  C07D309/30 ,  C07D311/86 ,  B01J2231/70 ,  B01J2531/845 ,  B01J31/2208

Abstract: An ether is oxidized with oxygen under an oxidation catalyst comprising an imide compound (such as N-hydroxyphthalimide) or the imide compound and a co-catalyst to produce the corresponding chain or cyclic ester or anhydride. The co-catalyst may be a transition metal compound. The above process provides a process for oxidizing an ether by oxygen efficiently to produce the corresponding oxide (such as an ester, an hydride) with high conversion and selectivity.

Abstract translation: 在包含酰亚胺化合物（例如N-羟基邻苯二甲酰亚胺）或酰亚胺化合物的氧化催化剂和助催化剂下，用氧氧化醚，以产生相应的链或环状酯或酸酐。 助催化剂可以是过渡金属化合物。 上述方法提供了通过氧气有效氧化醚的方法，以高转化率和选择性产生相应的氧化物（如酯，氢化物）。