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    • 2. 发明授权
    • Continuous preparation of polyamides from aminonitriles
    • 从氨基腈连续制备聚酰胺
    • US06316588B1
    • 2001-11-13
    • US09600957
    • 2000-07-25
    • Ralf MohrschladtVolker HildebrandtEberhard Fuchs
    • Ralf MohrschladtVolker HildebrandtEberhard Fuchs
    • C08G6900
    • C08G69/00C08G69/04C08G69/08C08G69/16C08G69/28C08K3/011
    • 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.
    • 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。
    • 5. 发明授权
    • Process for continuous purification of crude caprolactam prepared from
6-aminocapronitrile
    • 从6-氨基己腈制备的己内酰胺的连续纯化方法
    • US5496941A
    • 1996-03-05
    • US375410
    • 1995-01-18
    • Josef RitzRolf FischerWerner SchnurrGu/ nther AchhammerHermann LuykenEberhard Fuchs
    • Josef RitzRolf FischerWerner SchnurrGu/ nther AchhammerHermann LuykenEberhard Fuchs
    • C07D201/08C07D201/16
    • C07D201/16Y02P20/52
    • Crude capronitrile is purified by hydrogenation, subsequent treatment in an acidic medium and subsequent distillation in an alkaline medium, by a process in which(a) 6-aminocapronitrile is converted into crude caprolactam by reaction with water,(b) high boilers and low boilers are separated off from the crude caprolactam from step (a),(c) the crude caprolactam from step (b) is treated with hydrogen at from 50.degree. to 150.degree. C. and from 1.5 to 250 bar in the presence of a hydrogenation catalyst and, if desired, of a solvent to give a mixture A,(d1) mixture A in a solvent is passed, at from 30.degree. to 80.degree. C. and from 1 to 5 bar, over an ion exchanger containing terminal acid groups to give a mixture B1, or(d2) mixture A is distilled in the presence of sulfuric acid, any solvent present being removed before the addition of the sulfuric acid, to give a mixture B2, and(e) mixture B1 or mixture B2 is distilled in the presence of a base to give pure caprolactam.
    • 通过氢化纯化粗碳腈,随后在酸性介质中处理,随后在碱性介质中进行蒸馏,其中(a)通过与水反应将(a)6-氨基己腈转化为粗己内酰胺,(b)高锅炉和低锅炉 与步骤(a)中的粗己内酰胺分离,(c)步骤(b)中的粗己内酰胺在氢化催化剂存在下在50-150℃和1.5-250巴下用氢处理 并且如果需要,得到溶剂以得到混合物A,(d1)溶剂中的混合物A在30℃至80℃和1至5巴条件下通过含有末端酸基团的离子交换剂 得到混合物B1,或(d2)在硫酸存在下蒸馏混合物A,在加入硫酸之前,除去存在的任何溶剂,得到混合物B2,并且(e)蒸馏出混合物B1或混合物B2 在碱的存在下得到纯己内酰胺。
    • 6. 发明授权
    • Preparation of secondary and tertiary 2-methyl-1, 5-pentanediamines
    • 二级和叔级2-甲基-1,5-戊二胺的制备
    • US06198002B1
    • 2001-03-06
    • US09324715
    • 1999-06-03
    • Karsten EllerBernd FiegeStefan RittingerEberhard Fuchs
    • Karsten EllerBernd FiegeStefan RittingerEberhard Fuchs
    • C07C20948
    • C07C211/09C07C209/48
    • A process for preparing a secondary or tertiary 2-methyl-1,5-pen-tanediamine of the formula I where R1 and R2 are H, C1-C20-alkyl, C3-C8-cycloalkyl, aryl, C7-C20-arylalkyl, where the radicals R1 and R2 may bear substituents selected from the group consisting of C1-C20-alkyl, C1-C20-alkoxy, C6-C20-aryloxy and hydroxy, and R1 and R2 are not simultaneously hydrogen, or R1 and R2 are together an unsubstituted or C1-C20-alkyl- and/or C1-C20-alkoxy-substituted C3-C7-alkylene chain which may, if desired, be interrupted by one or two O or NR3 groups, where R3 is H or C1-C20-alkyl comprises reacting 2-methylglutarodinitrile with a primary or secondary amine of the formula R1R2NH and hydrogen at from 50 to 250° C. and pressures of from 0.5 to 35 MPa in the presence of an oxidic supported catalyst comprising one or more noble metals which has been treated with hydrogen at from 50 to 300° C. for at least 0.5 hour before use. The compound 1,5-bis(dimethylamino)-2-methylpentane is also claimed.
    • 制备式I其中R 1和R 2的仲或叔2-甲基-1,5-辛烷二胺的方法是H,C 1 -C 20 - 烷基,C 3 -C 8 - 环烷基,芳基,C 7 -C 20 - 芳烷基,其中 基团R 1和R 2可以具有选自C 1 -C 20 - 烷基,C 1 -C 20 - 烷氧基,C 6 -C 20 - 芳氧基和羟基的取代基,并且R 1和R 2不同时为氢,或者R 1和R 2一起为未取代或未取代的 C 1 -C 20烷基 - 和/或C 1 -C 20 - 烷氧基取代的C 3 -C 7 - 亚烷基链,如果需要,可以被一个或两个O或NR 3基团中断,其中R 3是H或C 1 -C 20烷基, - 甲基戊二腈与式R1R2NH的伯胺或仲胺和50-250℃的氢气和0.5-35MPa的压力在包含一种或多种已经用氢处理过的贵金属的氧化载体催化剂存在下 在使用前至少0.5小时,从50至300℃。 还要求化合物1,5-双(二甲基氨基)-2-甲基戊烷。
    • 10. 发明授权
    • Preparation of peralkylated amines
    • 全烷基化胺的制备
    • US5463130A
    • 1995-10-31
    • US395596
    • 1995-02-28
    • Tom WitzelEberhard FuchsHorst Zimmermann
    • Tom WitzelEberhard FuchsHorst Zimmermann
    • B01J23/44B01J23/58B01J23/63C07B61/00C07C209/48C07C209/60C07C211/09C07C213/02C07C215/08C08G18/18C08G59/68
    • C07C209/48C08G18/1808C08G18/1825C08G59/686
    • A process for the preparation of peralkylated amines of the general formula I ##STR1## in which R.sup.1, R.sup.2 denote C.sub.1 -C.sub.200 alkyl, C.sub.3 -C.sub.8 cycloalkyl, C.sub.4 -C.sub.20 alkylcycloalkyl, C.sub.4 -C.sub.20 cycloalkylalkyl, C.sub.2 -C.sub.20 alkoxyalkyl, aryl, C.sub.7 -C.sub.20 alkylaryl, C.sub.7 -C.sub.20 aralkyl, C.sub.2 -C.sub.8 hydroxyalkyl, C.sub.2 -C.sub.8 mercaptoalkyl, C.sub.8 -C.sub.20 phenoxyalkyl, C.sub.2 -C.sub.8 aminoalkyl, C.sub.2 -C.sub.8 (NHR.sup.4)alkyl, C.sub.2 -C.sub.8 (NR.sup.4 R.sup.5)alkyl or together form a saturated or unsaturated C.sub.2 -C.sub.6 alkylene chain optionally mono- to tri-substituted by C.sub.1 -C.sub.4 alkyl and optionally interrupted by oxygen or nitrogenX denotes a C.sub.2 -C.sub.20 alkylene or C.sub.2 -C.sub.20 alkenylene or C.sub.4 -C.sub.8 cycloalkylene chain optionally mono- to penta-substituted by R.sup.3, C.sub.1 -C.sub.8 alkyl, C.sub.1 -C.sub.8 alkoxy, C.sub.1 -C.sub.8 dialkylamino, phenoxy, diphenylamino and/or C.sub.2 -C.sub.8 alkoxycarbonyl,A denotes hydrogen, C.sub.1 -C.sub.20 alkyl, C.sub.3 -C.sub.8 cycloalkyl, C.sub.4 -C.sub.20 alkylcycloalkyl, C.sub.4 -C.sub.20 cycloalkylalkyl, C.sub.2 -C.sub.20 alkoxyalkyl, aryl, C.sub.7 -C.sub.20 alkylaryl, C.sub.7 -C.sub.20 aralkyl, C.sub.1 -C.sub.20 alkoxy, hydroxy, C.sub.1 -C.sub.20 hydroxyalkyl, amino, C.sub.1 -C.sub.20 alkylamino, C.sub.2 -C.sub.20 dialkylamino, C.sub.3 -C.sub.12 alkenyleneamino, C.sub.3 -C.sub.8 cycloalkylamino, arylamino, aryl-C.sub.1 -C.sub.12 alkylamino, halogen, mercapto, C.sub.2 -C.sub.20 alkenylenoxy, C.sub.3 -C.sub.8 cycloalkoxy and aryloxyR.sup.3 denotes CH.sub.2 --NR.sup.1 R.sup.2,R.sup.4, R.sup.5 denote C.sub.1 -C.sub.20 alkylby the reaction of a nitrile of the general formula IIA--X--CN (II),in which R.sup.1, R.sup.2, R.sup.4, R.sup.5, X and A have the aforementioned meanings and R.sup.3 stands for --CH.sub.2 --NR.sup.1 R.sup.2 or cyano, with a secondary amine of the general formula III ##STR2## and hydrogen at temperatures ranging from 50.degree. to 250.degree. C. and pressures ranging from 5 to 350 bar in the presence of a catalyst, wherein the catalyst used is palladium on an oxidic support.
    • 制备通式I(I)的全烷基胺的方法,其中R 1,R 2表示C 1 -C 20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,C 2 -C 20烷氧基烷基,芳基,C 7 -C 20烷基芳基 C 7 -C 20烷基,C 2 -C 8羟烷基,C 2 -C 8巯基烷基,C 8 -C 20苯氧烷基,C 2 -C 8氨基烷基,C 2 -C 8(NHR 4)烷基,C 2 -C 8(NR 4 R 5)烷基或一起形成饱和或不饱和的C 2 -C 6亚烷基链, 被C1-C4烷基三取代并且任选地被氧或氮中断X表示任选被R 3,C 1 -C 8烷基,C 1 -C 8烷氧基,C 1 -C 8烷氧基取代的C 2 -C 20亚烷基或C 2 -C 20亚烯基或C 4 -C 8亚烷基链, C 2 -C 20烷基氨基,苯氧基,二苯基氨基和/或C 2 -C 8烷氧基羰基,A表示氢,C 1 -C 20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,C 2 -C 20烷氧基烷基,芳基,C 7 -C 20烷基芳基,C 7 -C 20芳烷基,C 1 -C 20烷氧基, 羟基,C 1 -C 20羟烷基,氨基,C 1 -C 20烷基氨基,C 2 -C 20二烷基氨基,C 3 -C 12亚烯基氨基, C 3 -C 8环烷基氨基,芳基氨基,芳基-C 1 -C 12烷基氨基,卤素,巯基,C 2 -C 20烯基烯氧基,C 3 -C 8环烷氧基和芳氧基R 3表示CH 2 -NR 1 R 2,R 4,R 5表示通过通式II的腈反应的C 1 -C 20烷基 -CN(II),其中R1,R2,R4,R5,X和A具有上述含义,R3代表-CH2-NR1R2或氰基,与通式III的仲胺(III)和 氢气在50至250℃的温度和5至350巴的压力范围内,在催化剂存在下,其中使用的催化剂是氧化载体上的钯。