公开(公告)号：US06316588B1

公开(公告)日：2001-11-13

申请号：US09600957

申请日：2000-07-25

Applicant: Ralf Mohrschladt ,  Volker Hildebrandt ,  Eberhard Fuchs

Inventor： Ralf Mohrschladt ,  Volker Hildebrandt ,  Eberhard Fuchs

IPC: C08G6900

CPC classification number: C08G69/00 ,  C08G69/04 ,  C08G69/08 ,  C08G69/16 ,  C08G69/28 ,  C08K3/011

Abstract: A continuous process for preparing a polyamide by reacting at least one aminonitrile with water comprises: (1) reacting at least one aminonitrile with water at a temperature from 90 to 400° C. and a pressure from 0.1 to 35×106 Pa in a flow tube containing a Brönsted acid catalyst selected from a beta-zeolite catalyst, a sheet-silicate catalyst or a titanium dioxide catalyst comprising from 70 to 100% by weight of anatase and from 0 to 30% by weight of rutile and in which up to 40% by weight of the titanium dioxide may be replaced by tungsten oxide to obtain a reaction mixture, (2) further reacting the reaction mixture at a temperature from 150 to 400° C. and a pressure which is lower than the pressure in step 1, in the presence of a Brönsted acid catalyst as in (1), the temperature and pressure being selected so as to obtain a first gas phase and a first liquid or a first solid phase or a mixture of first solid and first liquid phase, and the first gas phase is separated from the first liquid or the first solid phase or from the mixture of first liquid and first solid phase, and (3) admixing the first liquid or the first solid phase or the mixture of first liquid and first solid phase with a gaseous or liquid phase comprising water at a temperature from 150 to 370° C. and a pressure from 0.1 to 30×106 Pa to obtain a product mixture.

Abstract translation: 通过使至少一种氨基腈与水反应制备聚酰胺的连续方法包括：（1）在90-400℃的温度和0.1至35×10 6 Pa的压力下使至少一种氨基腈与水反应， 选自β-沸石催化剂，片状硅酸盐催化剂或二氧化钛催化剂的布朗斯台德酸催化剂，其包含70至100重量％的锐钛矿和0至30重量％的金红石，其中至多40重量％ 二氧化钛的重量可以被氧化钨代替以获得反应混合物，（2）使反应混合物在150-400℃的温度和低于步骤1的压力的压力下反应，在 存在如（1）中所述的布朗斯台德酸催化剂，选择温度和压力以获得第一气相和第一液体或第一固相或第一固体和第一液相的混合物，并且第一气体 相与杉木分离 第一液体或第一固相或第一液体和第一固相的混合物，和（3）将第一液体或第一固相或第一液体和第一固相的混合物与包含水的气相或液相混合 温度为150〜370℃，压力为0.1〜30×10 6 Pa，得到产物混合物。

公开(公告)号：US06222033B1

公开(公告)日：2001-04-24

申请号：US09403655

申请日：1999-10-25

Applicant: Eberhard Fuchs ,  Rolf Fischer

Inventor： Eberhard Fuchs ,  Rolf Fischer

IPC: C07D20108

CPC classification number: C07D201/08

Abstract: The disclosure is a process for preparing cyclic lactams of the formula I: where R1 is hydrogen, alkyl, cycloalkyl or aryl, and A is C3-C12-alkylene unsubstituted or substituted by 1, 2, 3, 4, 5 or 6 substituents selected independently of one another from the group consisting of alkyl, cycloalkyl and aryl, by conversion of an &ohgr;-aminocarbonitrile of the formula II: HR1N—A—CN  (II) where R1 and A are each as defined above, in the presence of at least one catalyst, which comprises converting said nitrile II into an oligomer mixture, and treating with superheated steam.

Abstract translation: 本公开是制备式I的环状内酰胺的方法：其中R 1是氢，烷基，环烷基或芳基，A是未被取代或被1,2,3,4,5或6个取代基取代的C 3 -C 12亚烷基， 通过在至少一种催化剂的存在下，通过转化式II的ω-氨基腈（其中R 1和A各自如上所定义），其中包括将所述腈II 进入低聚物混合物，并用过热蒸汽处理。

公开(公告)号：US6147208A

公开(公告)日：2000-11-14

申请号：US91130

申请日：1998-06-16

Applicant: Gunther Achhammer ,  Peter Bassler ,  Rolf Fischer ,  Eberhard Fuchs ,  Hermann Luyken ,  Werner Schnurr ,  Guido Voit ,  Lutz Hilprecht

Inventor： Gunther Achhammer ,  Peter Bassler ,  Rolf Fischer ,  Eberhard Fuchs ,  Hermann Luyken ,  Werner Schnurr ,  Guido Voit ,  Lutz Hilprecht

IPC: C07C209/48 ,  C07C209/86 ,  C07C211/12 ,  C07D201/08 ,  C07D201/02

CPC classification number: C07D201/08 ,  C07C209/48 ,  Y02P20/52

Abstract: Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile.

Abstract translation: PCT No.PCT / EP96 / 05521 Sec。 371日期：1998年6月16日 102（e）日期1998年6月16日PCT 1996年12月11日PCT公布。 公开号WO97 / 23454 日期1997年7月3日由己二腈起始制备己内酰胺和六亚甲基二胺。

公开(公告)号：US6002010A

公开(公告)日：1999-12-14

申请号：US952239

申请日：1997-11-10

Applicant: Eberhard Fuchs

Inventor： Eberhard Fuchs

IPC: C07D213/79 ,  C07B61/00 ,  C07C67/22 ,  C07C69/34 ,  C07C231/06 ,  C07C233/02 ,  C07D213/80 ,  C07D213/803 ,  C07D213/81 ,  C07D213/84 ,  C07D213/56

CPC classification number: C07D213/803 ,  C07C231/06 ,  C07C67/22 ,  C07D213/80 ,  C07D213/81

Abstract: A process for preparing carboxylic acid derivatives of the formula I ##STR1## where X is OR.sup.2 or NH.sub.2,R.sup.1 is C.sub.1 -C.sub.20 -alkyl, C.sub.l -C.sub.20 -hydroxyalkyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.4 -C.sub.12 -alkylcycloalkyl, C.sub.4 -C.sub.12 -cycloalkylalkyl, C.sub.5 -C.sub.20 -alkylcycloalkylalkyl, aryl, C.sub.7 -C.sub.20 -aralkyl, C.sub.7 -C.sub.20 -alkylaryl, a heteroaliphatic or heteroaromatic ring with 5 to 8 carbon atoms andR.sup.2 is C.sub.1 -C.sub.20 -alkyl,from carbonitriles of the formula IIR.sup.1 --C.tbd.N (II),where R.sup.1 has the abovementioned meanings, and alcohols of the formula IIIR.sup.2 --OH (III),where R.sup.2 has the abovementioned meanings, at from 50 to 300.degree. C. under from 0.1 to 350 bar in the presence of a heterogeneous catalyst, wherein the reaction is carried out in liquid phase.

Abstract translation: PCT No.PCT / EP96 / 01890 Sec。 371日期：1997年11月10日 102（e）1997年11月10日日期PCT提交1996年5月7日PCT公布。 第WO96 / 36592号公报 日期：1996年11月21日制备式I的羧酸衍生物的方法，其中X是OR 2或NH 2，R 1是C 1 -C 20烷基，C 1 -C 20羟烷基，C 3 -C 12环烷基，C 4 -C 12烷基环烷基，C 4 C 12 - 环烷基烷基，C 5 -C 20 - 烷基环烷基烷基，芳基，C 7 -C 20 - 芳烷基，C 7 -C 20烷基芳基，具有5至8个碳原子的杂脂族或杂芳族环，R 2为C 1 -C 20 - 烷基， IIR1-C 3BOND N（II）其中R1具有上述含义，和式IIIR2-OH（III）的醇，其中R2具有上述含义，在50至300℃，0.1至350巴 存在非均相催化剂，其中反应在液相中进行。

公开(公告)号：US5894074A

公开(公告)日：1999-04-13

申请号：US50918

申请日：1998-03-31

Applicant: Eberhard Fuchs ,  Boris Breitscheidel ,  Rainer Becker ,  Horst Neuhauser

Inventor： Eberhard Fuchs ,  Boris Breitscheidel ,  Rainer Becker ,  Horst Neuhauser

IPC: B01J23/44 ,  C07B61/00 ,  C07C209/48 ,  C07C211/09 ,  C07C213/02 ,  C07C215/08

CPC classification number: C07C213/02 ,  C07C209/48

Abstract: A process for preparing amines of the general formula (I)X(--CH.sub.2 --NR.sup.1 R.sup.2).sub.n (I)whereR.sup.1 and R.sup.2 are preferably methyl, X is preferably 1,4-butylene and n is preferably 2, comprises reacting nitriles of the general formula (II)(R.sup.1 R.sup.2 N--CH.sub.2 --).sub.n-m X(--CN).sub.m (II)where R.sup.1, R.sup.2 and X are each as defined above and m is an integer from 1 to n,with secondary amines of the general formula (III)HNR.sup.1 R.sup.2 (III)where R.sup.1 and R.sup.2 are each as defined above,and hydrogen at from 50 to 250.degree. C. and from 5 to 350 bar in the presence of a palladium catalyst comprising, based on the total weight of the catalyst, from 0.1 to 10% by weight of Pd and from 0.01 to 10% by weight of at least one further metal selected from groups IB and VII of the Periodic Table, cerium and lanthanum on a support.

Abstract translation: 其中R1和R2优选为甲基，X优选为1,4-丁烯并且n优选为2的制备通式（I）X（-CH 2 -NR 1 R 2）n（I）的胺的方法包括使 通式（II）（R1R2N-CH2-）n-mX（-CN）m（II）其中R1，R2和X各自如上所定义，m是1至n的整数，通式 （III）其中R 1和R 2各自如上定义的HNR1R2（III）和在钯催化剂存在下在50-250℃和5-35巴条件下的氢气，其包含基于催化剂总重量 ，0.1至10重量％的Pd和0.01至10重量％的选自元素周期表中的IB和VII族的至少一种其它金属，铈和镧在载体上。

公开(公告)号：US5557011A

公开(公告)日：1996-09-17

申请号：US339916

申请日：1994-11-15

Applicant: Tom Witzel ,  Eberhard Fuchs

Inventor： Tom Witzel ,  Eberhard Fuchs

IPC: B01J23/44 ,  C07B61/00 ,  C07C209/48 ,  C07C211/09

CPC classification number: C07C209/48

Abstract: Process for the preparation of diamines of the general formula I ##STR1## in which A denotes a C.sub.1 -C.sub.20 alkylene chain optionally mono- to penta-substituted by C.sub.1 -C.sub.4 alkyl,R.sup.1, R.sup.2 denote C.sub.1 -C.sub.20 alkyl, C.sub.1 -C.sub.20 hydroxyalkyl, C.sub.3 -C.sub.8 cycloalkyl, C.sub.4 -C.sub.20 alkylcycloalkyl, C.sub.4 -C.sub.20 cycloalkylalkyl, phenyl, C.sub.7 -C.sub.20 phenylalkyl, C.sub.1 -C.sub.20 alkoxyalkyl, C.sub.7 -C.sub.20 phenoxyalkyl or together a saturated or unsaturated C.sub.2 -C.sub.6 alkylene chain optionally monosubstituted, disubstituted, or trisubstituted by C.sub.1 -C.sub.4 alkyl and optionally interrupted by oxygen or nitrogen,by the reaction of dinitriles of the general formula IINC--A--CN (II),in which A has the aforementioned meaning,with secondary amines of the general formula II ##STR2## in which R.sup.1 and R.sup.2 have the aforementioned meanings, with hydrogen at temperatures ranging from 50.degree. to 200.degree. C. and pressures ranging from 5 to 300 bar in the presence of a hydrogenation catalyst, in which a palladium catalyst on an oxidic support is used as hydrogenation catalyst.

Abstract translation: 制备通式I（II）的二胺的方法，其中A表示任选被C 1 -C 4烷基单取代至五取代的C 1 -C 20亚烷基链，R 1，R 2表示C 1 -C 20烷基，C 1 -C 20羟基烷基，C 3 -C 8环烷基，C 4 -C 20烷基环烷基，C 4 -C 20环烷基烷基，苯基，C 7 -C 20苯基烷基，C 1 -C 20烷氧基烷基，C 7 -C 20苯氧基烷基或一起饱和或不饱和的C 2 -C 6亚烷基链，任选单取代，二取代 或通过C 1 -C 4烷基三取代并且任选地被氧或氮中断，通过其中A具有上述含义的通式IINC-A-CN（II）的二腈与通式II的仲胺反应， 其中R 1和R 2具有上述含义，在氢化催化剂存在下，在氢气温度范围为50-200℃，压力范围为5-300巴，其中钯催化剂 在氧化载体上用作氢化催化剂 t。

公开(公告)号：US5495016A

公开(公告)日：1996-02-27

申请号：US358411

申请日：1994-12-19

Applicant: Gunther Achhammer ,  Eberhard Fuchs

Inventor： Gunther Achhammer ,  Eberhard Fuchs

IPC: C07D201/08 ,  C07D223/10

CPC classification number: C07D201/08 ,  Y02P20/584

Abstract: Caprolactam is prepared by reacting a solution of 6-aminocapronitrile with water in the liquid phase at elevated temperatures by a process in which(a) an aqueous solution of 6-aminocapronitrile in the liquid phase is heated without the addition of a catalyst in a reactor A to give a mixture I consisting essentially of water, caprolactam and a high-boiling fraction (high boiler), then(b) the water is removed from the resulting mixture I to give a mixture II consisting essentially of caprolactam and the high boilers, then(c) the caprolactam and the high boilers from mixture II are separated from one another by distillation, and then either(d1) the high boilers from stage (c) are fed into the reactor A of stage (a) or(d2) the high boilers are heated similarly to stage (a) in a further reactor B and then worked up similarly to stages (b) and (c) to give further caprolactam, or(d3) the high boilers are heated under reduced pressure in the presence of a base in a reactor C and the reacted mixture is worked up by distillation to give caprolactam.

Abstract translation: 己内酰胺通过以下方法制备：在高温下使6-氨基己腈与水在液相中反应，其中（a）将液相中的6-氨基己腈水溶液加热而不在反应器中加入催化剂 A得到基本上由水，己内酰胺和高沸点馏分（高锅炉）组成的混合物I，然后（b）从所得混合物I中除去水，得到基本上由己内酰胺和高锅炉组成的混合物II， 然后（c）通过蒸馏将己内酰胺和来自混合物II的高沸点物彼此分离，然后（d1）将来自阶段（c）的高沸点物（d）进料到步骤（a）或（d2）的反应器A中， 类似于在另一个反应器B中的阶段（a）类似地加热高锅炉，然后类似于阶段（b）和（c）进行加工以得到进一步的己内酰胺，或（d3）在存在下在减压下加热高锅炉 的反应器C和反应器中的碱 通过蒸馏处理混合物以得到己内酰胺。

公开(公告)号：US5481037A

公开(公告)日：1996-01-02

申请号：US299065

申请日：1994-08-31

Applicant: Eberhard Fuchs ,  Tom Witzel ,  Klaus P. Stadler

Inventor： Eberhard Fuchs ,  Tom Witzel ,  Klaus P. Stadler

IPC: C07C209/84 ,  C07C211/12 ,  C07C211/35 ,  C07C209/86

CPC classification number: C07C209/84 ,  C07C2101/14

Abstract: A process for the purification of tertiary amines in a crude mixture contaminated with undesirable primary and secondary amines which may have only a slight variance in boiling point with respect to the tertiary amine, wherein the crude mixture of the tertiary amine is treated at temperatures which may range from 0.degree. to 200.degree. C. but preferably from 20 to 150.degree. C. and at pressures of from 1 to 200 bar but most preferably under atmospheric pressure with a carboxylate of the formula ##STR1## in which R.sup.4 and R.sup.5 are selected from the group consisting of C.sub.1 -C.sub.20 -alkyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.4 -C.sub.20 -cycloalkylalkyl, and aryl or C.sub.7 -C.sub.20 -aralkyl, both optionally mono- to penta- substituted by C.sub.1 -C.sub.8 -alkyl, C.sub.3 -C.sub.8 -cycloalkyl, or C.sub.4 -C.sub.12 -cycloalkylalkyl, and R.sup.4 may also represent hydrogen,to selectively form the alkylamides of the primary and secondary amine contaminants; and then separating the alkylamides from the tertiary amine by distillation.

Abstract translation: 在不合适的伯胺和仲胺污染的粗混合物中纯化叔胺的方法，其可能在叔胺方面可能只有轻微的沸点变化，其中叔胺的粗混合物在 在0至200℃范围内，优选20至150℃，压力范围为1至200巴，最优选在大气压下，使用其中选择R 4和R 5的羧酸酯 由C 1 -C 20 - 烷基，C 3 -C 12 - 环烷基，C 4 -C 20 - 环烷基烷基和芳基或C 7 -C 20 - 芳烷基组成的组，任选被C 1 -C 8 - 烷基，C 3 -C 8 环烷基或C 4 -C 12环烷基烷基，并且R 4也可以代表氢，以选择性地形成伯胺和仲胺污染物的烷基酰胺; 然后通过蒸馏将烷基酰胺与叔胺分离。

公开(公告)号：US06683179B2

公开(公告)日：2004-01-27

申请号：US10258941

申请日：2002-10-29

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

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

IPC: C07D20108

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）在催化剂存在下在气相中反应，得到含己内酰胺，氨，水的混合物（II） ，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）然后将水 从混合物（III）中除去，得到含有己内酰胺，高沸点组分和低沸点组分的混合物（IV），然后通过结晶从混合物（IV）获得含有己内酰胺的固体（V），比例 的固体（V）中的己内酰胺的量大于混合物（IV）中的。

公开(公告)号：US06677449B2

公开(公告)日：2004-01-13

申请号：US10258942

申请日：2002-10-29

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

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

IPC: C07D20102

CPC classification number: C07D201/08 ,  C07D201/16

Abstract: A process for the preparation of caprolactam is provided, wherein a) a mixture (I) containing 6-aminocapronitrile and water is reacted in the liquid 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）在液相中在催化剂存在下反应，得到含有己内酰胺，氨，水的混合物（II） ，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）然后将水 从混合物（III）中除去，得到含有己内酰胺，高沸点组分和低沸点组分的混合物（IV），然后通过结晶从混合物（IV）获得含有己内酰胺的固体（V），比例 的固体（V）中的己内酰胺的量大于混合物（IV）中的。