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    • 1. 发明授权
    • Preparation of amines and aminonitriles
    • 胺和氨基腈的制备
    • US5789621A
    • 1998-08-04
    • US693983
    • 1996-08-08
    • Werner SchnurrGuido VoitKlemens FlickRolf-Hartmuth Fischer
    • Werner SchnurrGuido VoitKlemens FlickRolf-Hartmuth Fischer
    • B01J23/78B01J23/94B01J27/187B01J27/28B01J38/10C07B43/04C07B61/00C07C20060101C07C209/48C07C209/52C07C211/12C07C211/35C07C253/30C07C255/24C07C209/02
    • C07C209/48C07C209/52
    • A process for preparing an NH.sub.2 -containing compound by hydrogenating a compound containing at least one unsaturated carbon-nitrogen bond with hydrogen in the presence of a catalyst at temperatures not below room temperature and elevated hydrogen partial pressure in the presence or absence of a solvent which process includes the following steps: a) using a catalyst comprising a cobalt- and/or iron-containing catalyst, and b) after the conversion based on the compound to be hydrogenated and/or the selectivity based on the desired product has or have dropped below a defined value or the amount of an unwanted by-product has risen beyond a defined value, interrupting the hydrogenation by stopping the feed of the compound to be hydrogenated and of the solvent, if used, c) treating the catalyst at from 150.degree. to 400.degree. C. with hydrogen using a hydrogen pressure within the range from 0.1 to 30 MPa and a treatment time within the range from 2 to 48 h, and d) subsequently continuing the hydrogenation of the compound containing at least one unsaturated carbon-nitrogen bond.
    • 在催化剂存在下,在不低于室温和升高的氢分压的情况下,在存在或不存在溶剂的情况下,通过氢化含有至少一个不饱和碳 - 氮键的化合物与氢气来制备含NH 2的化合物的方法, 方法包括以下步骤:a)使用包含含钴和/或含铁催化剂的催化剂,和b)基于待氢化的化合物转化后,和/或基于所需产物的选择性具有或已经下降 低于定义的值或不想要的副产物的量已经超过定义的值,如果使用,则通过停止待氢化化合物的进料和溶剂的中断氢化,c)在150℃下处理催化剂 在氢气压力为0.1〜30MPa,处理时间为2〜48h的范围内,使氢气变为400℃,d)随后继续进行水压 该化合物含有至少一个不饱和碳 - 氮键。
    • 7. 发明授权
    • Method for reducing the content of an unsaturated amine in a mixture containing an amino nitrile, a diamine, a dinitrile or mixtures thereof
    • 降低含氨基腈,二胺,二腈或其混合物的混合物中不饱和胺含量的方法
    • US07385073B2
    • 2008-06-10
    • US10515281
    • 2003-05-21
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BaβlerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • Stefan MaixnerChristoph BenischHermann LuykenPeter BaβlerRolf-Hartmuth FischerJohann-Peter MelderAndreas Ansmann
    • C07C253/34
    • C07C253/34C07C255/24
    • A process for reducing the level of an aliphatic monounsaturated amine (IV) in a mixture (V) containing an aminonitrile (I) or a diamine (II) or a dinitrile (III) or mixtures thereof as well as said mine (IV) by a) reacting said mixture (V) with an anionic nucleophile (VI) which contains a nucleophilic atom selected from the group consisting of oxygen, nitrogen and sulfur, which is capable of taking up an H+ ion to form an acid having a pKa value in the range from 7 to 11, as measured in water at 25° C., and which has a relative nucleophilicity, as measured in methyl perchlorate/methanol at 25° C., in the range from 3.4 to 4.7 when said nucleophilic atom is oxygen, in the range from 4.5 to 5.8 when said nucleophilic atom is nitrogen, and in the range from 5.5 to 6.8 when said nucleophilic atom is sulfur, in an amount in the range from 0.01 to 10 mol per mole of said amine (IV) in said mixture (V) at a temperature in the range from 50 to 200° C. to obtain a mixture (VII), b) distilling said aminonitrile (I) or said diamine (II) or said dinitrile (III) or mixtures thereof from said mixture (VII) at a temperature in the range from 50 to 200° C. and at a pressure in the range from 0.1 to 100 kPa to obtain a bottom product (VIII), which comprises c) distilling an aminonitrile (I) or diamine (II) or dinitrile (III) or mixtures thereof from said bottom product (VIII) at a temperature which is lower than that chosen in step b).
    • 在含有氨基腈(I)或二胺(II)或二腈(III)或其混合物以及所述矿(IV)的混合物(V)中降低脂族单不饱和胺(IV)的水平的方法, a)使所述混合物(V)与阴离子亲核试剂(VI)反应,所述阴离子亲核试剂(VI)含有选自氧,氮和硫的亲核原子,其能够吸收H + 形成在25℃下在水中测量的具有7至11的pK值的酸,其在25℃下在高氯酸甲酯/甲醇中测得的具有相对亲核性 当所述亲核原子为氧时,在3.4至4.7的范围内,当所述亲核原子为氮时,在4.5至5.8的范围内,当所述亲核原子为硫时在5.5至6.8的范围内,其量为 在所述混合物(V)中在50至200℃的温度范围内每摩尔所述胺(IV)为0.01至10摩尔的范围,以获得混合物 (VII)中,b)在50至200℃的温度下,从所述混合物(VII)中蒸馏所述氨基腈(I)或所述二胺(II)或所述二腈(III)或其混合物, 压力为0.1至100kPa,以获得底部产物(VIII),其包括c)在所述底部产物(VIII)中蒸馏氨基腈(I)或二胺(II)或二腈(III)或其混合物, 温度低于步骤b)中选择的温度。
    • 10. 发明授权
    • Method for the production of 1,4- butane-diol by combined gas-phase and liquid-phase hydrogenation
    • 通过组合气相和液相氢化生产1,4-丁二醇的方法
    • US07169958B2
    • 2007-01-30
    • US10516923
    • 2003-06-10
    • Michael HesseStephan SchlitterHolger BorchertMarkus SchubertMarkus RöschNils BottkeRolf-Hartmuth FischerAlexander WeckGunther WindeckerGunnar Heydrich
    • Michael HesseStephan SchlitterHolger BorchertMarkus SchubertMarkus RöschNils BottkeRolf-Hartmuth FischerAlexander WeckGunther WindeckerGunnar Heydrich
    • C07C29/132C07C29/149C07C29/136C07C29/147
    • C07C29/149C07C31/207
    • The present invention relates to a process for preparing optionally alkyl-substituted 1,4-butanediol by two-stage catalytic hydrogenation in the gas phase of C4-dicarboxylic acids and/or of derivatives thereof having the following steps: a) introducing a gas stream of a C4-dicarboxylic acid or of a derivative thereof at from 200 to 300° C. and from 2 to 60 bar into a first reactor and catalytically hydrogenating it to a product which contains mainly optionally alkyl-substituted γ-butyrolactone; b) converting the product stream into the liquid phase; c) introducing the product stream obtained in this way into a second reactor at a temperature of from 100° C. to 240° C. and a pressure of from 20 to 250 bar and catalytically hydrogenating it in the liquid phase to optionally alkyl-substituted 1,4-butanediol; d) removing the desired product from by-products and any unconverted reactants; e) optionally recycling unconverted intermediates into one or both hydrogenation stages, said hydrogenation stages both using a catalyst which comprises ≦95% by weight, preferably from 5 to 95% by weight, in particular from 10 to 80% by weight, of CuO, and ≧5% by weight, preferably from 5 to 95% by weight, in particular from 20 to 90% by weight, of a support, said second reactor having a higher pressure than said first reactor, and the product mixture removed from said first reactor being introduced without further purification into said second reactor.
    • 本发明涉及通过在具有下列物质的C 4 - 二羧酸和/或其衍生物的气相中通过两阶段催化氢化制备任选的烷基取代的1,4-丁二醇的方法 步骤:a)将200-300℃和2-60巴的C 4-14二羧酸或其衍生物的气流引入第一反应器,并将其催化氢化至 主要含烷基取代的γ-丁内酯的产品; b)将产物流转化成液相; c)将以这种方式获得的产物流在100℃至240℃的温度和20至250巴的压力下引入第二反应器,并将其在液相中催化氢化为任选的烷基取代的 1,4-丁二醇 d)从副产物和任何未转化的反应物中除去所需的产物; e)任选地将未转化的中间体再循环到一个或两个氢化阶段中,所述氢化步骤均使用包含<= 95重量%,优选5至95重量%,特别是10至80重量%的CuO ,和> = 5重量%,优选5至95重量%,特别是20至90重量%的载体,所述第二反应器具有比所述第一反应器更高的压力,并将产物混合物从 所述第一反应器不经进一步纯化地引入所述第二反应器。