Method for the production of defined mixtures of thf, bdo and gbl by gas phase hydrogenation

    公开(公告)号:US20070135650A1

    公开(公告)日:2007-06-14

    申请号:US10581074

    申请日:2004-12-04

    IPC分类号: C07D307/02

    CPC分类号: C07D307/33 C07D307/08

    摘要: The present invention provides a process for variably preparing mixtures of optionally alkyl-substituted BDO, GBL and THF by two-stage hydrogenation in the gas phase of C4 dicarboxylic acids and/or derivatives thereof, which comprises a) in a first step in the gas phase, hydrogenating a gas stream of C4 dicarboxylic acids and/or derivatives thereof over a catalyst at a pressure of from 2 to 100 bar and a temperature of from 200° C. to 300° C. in a first reactor in the presence of a catalyst in the form of shaped catalyst bodies having a volume of less than 20 mm3, said catalyst from 5 to 95% by weight of oxide of copper and from 5 to 95% by weight of an oxide having acidic sites, to give a stream mainly containing of optionally alkyl-substituted GBL and THF, b) removing any succinic anhydride formed by partial condensation, c) converting the products remaining predominantly in the gas phase in the partial condensation, THF, water and GBL, under the same pressure or under a pressure reduced by the pressure drops in the hydrogenation circuit and at a temperature of from 150 to 240° C., in a second reactor over a catalyst which ≦95% by weight of CuO and from 5 to 95% by weight of one or more oxides selected from the group of ZnO, Al2O3, SiO2, TiO2, ZrO2, CeO2, MgO, CaO, SrO, BaO, La2O3 and Mn2O3 to give a stream comprising a mixture of BDO, GBL and THF, d) removing the hydrogen from the products and recycling it into the hydrogenation, e) distillatively separating the products, THF, BDO, GBL and water, if appropriate recycling a GBL-rich stream into the second reactor or if appropriate discharging it, and working up BDO, THF and GBL distillatively, and setting the ratio of the products, THF, GBL and BDO, relative to one another within the range from 10 to 100% by weight of THF, from 0 to 90% by weight of GBL and from 0 to 90% by weight of BDO only by varying the temperatures in the two hydrogenation zones and also if appropriate the GBL recycle stream.

    Method for the production of defined mixtures of THF, BDO and GBL by gas phase hydrogenation
    5.
    发明授权
    Method for the production of defined mixtures of THF, BDO and GBL by gas phase hydrogenation 失效
    通过气相氢化制备THF,BDO和GBL的限定混合物的方法

    公开(公告)号:US07442810B2

    公开(公告)日:2008-10-28

    申请号:US10581074

    申请日:2004-12-04

    IPC分类号: C07D307/00 C07D307/02

    CPC分类号: C07D307/33 C07D307/08

    摘要: A process for variably preparing mixtures of optionally alkyl-substituted BDO, GBL and THF by two-stage hydrogenation in the gas phase of C4 dicarboxylic acids and/or derivatives thereof, which comprises a) hydrogenating in a gas phase a gas stream of C4 dicarboxylic acids and/or derivatives thereof over a particular catalyst at a particular pressure and temperature to give a stream mainly containing of optionally alkyl-substituted GBL and THF, b) removing any succinct anhydride, c) converting the products remaining predominantly in the gas phase in the partial condensation, THF, water and GBL to give a stream comprising a mixture of BDO, GBL and THF, d) removing the hydrogen from the products and recycling it into the hydrogenation, e) distillatively separating the products, THF, BDO, GBL and water, if appropriate recycling a GBL-rich stream or if appropriate discharging it, and working up BDO, THF and GBL distillatively, and setting the ratio of the products, THF, GBL and BDO, relative to one another within the range from 10 to 100% by weight of THF, from 0 to 90% by weight of GBL and from 0 to 90% by weight of BDO only by varying the temperatures in the two hydrogenation zones and also if appropriate the GBL recycle stream.

    摘要翻译: 一种在可能地制备任选烷基取代的BDO,GBL和THF的混合物的方法,其通过在C 4 C 4羧酸和/或其衍生物的气相中进行两步氢化,其包括a)在 在特定的压力和温度下,将特定催化剂上的C 4 O 2羧酸和/或其衍生物的气流气相,得到主要含有烷基取代的GBL和THF的物流,b)除去 任何简单的酸酐,c)将部分冷凝,THF,水和GBL中主要保留在气相中的产物进行转化,得到包含BDO,GBL和THF的混合物的流,d)从产物中除去氢并将其再循环 进入氢化,e)蒸馏分离产物,THF,BDO,GBL和水,如果适当回收富含GBL的物流或适当排放,并蒸馏处理BDO,THF和GBL,并设定产物的比例 ,TH F,GBL和BDO相对于10重量%至100重量%的THF,0至90重量%的GBL​​和0至90重量%的BDO,仅通过改变两者中的温度 加氢区,如果合适的话也可以使用GBL再循环流。

    Method for the Recovery of Ruthenium From Used Ruthenium Oxide-Containing Catalysts
    8.
    发明申请
    Method for the Recovery of Ruthenium From Used Ruthenium Oxide-Containing Catalysts 有权
    从使用的含氧化钌催化剂中回收钌的方法

    公开(公告)号:US20080293836A1

    公开(公告)日:2008-11-27

    申请号:US12158085

    申请日:2006-12-21

    IPC分类号: C07C27/00

    摘要: The invention relates to a process for recovering ruthenium from a used ruthenium-comprising catalyst which comprises ruthenium as ruthenium oxide on a support material which is sparingly soluble in mineral acid, which comprises the steps: a) the catalyst comprising ruthenium oxide is treated in a stream of hydrogen, with ruthenium oxide present on the support being reduced to metallic ruthenium; b) the reduced catalyst from step a) comprising metallic ruthenium on the support material is treated with hydrochloric acid in the presence of an oxygen-comprising gas, with the metallic ruthenium present on the support being dissolved as ruthenium(III) chloride and being obtained as ruthenium(III) chloride solution; c) if appropriate, the ruthenium(III) chloride solution from step b) is worked up further.

    摘要翻译: 本发明涉及一种用于从使用的含钌催化剂中回收钌的方法,其中将钌作为氧化钌在微溶于无机酸的载体材料上包括以下步骤:a)将包含氧化钌的催化剂在 存在于载体上的氧化钌还原成金属钌; b)在载体材料上包含金属钌的步骤a)的还原催化剂在含氧气体存在下用盐酸处理,载体上存在的金属钌以氯化钌(III)的形式溶解并得到 作为氯化钌(III)溶液; c)如果合适,将步骤b)的氯化钌(III)溶液进一步处理。

    Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts
    10.
    发明授权
    Method for the recovery of ruthenium from used ruthenium oxide-containing catalysts 有权
    从使用的含氧化钌催化剂中回收钌的方法

    公开(公告)号:US07704469B2

    公开(公告)日:2010-04-27

    申请号:US12158085

    申请日:2006-12-21

    IPC分类号: C22B11/00

    摘要: The invention relates to a process for recovering ruthenium from a used ruthenium-comprising catalyst which comprises ruthenium as ruthenium oxide on a support material which is sparingly soluble in mineral acid, which comprises the steps: a) the catalyst comprising ruthenium oxide is treated in a stream of hydrogen, with ruthenium oxide present on the support being reduced to metallic ruthenium; b) the reduced catalyst from step a) comprising metallic ruthenium on the support material is treated with hydrochloric acid in the presence of an oxygen-comprising gas, with the metallic ruthenium present on the support being dissolved as ruthenium(III) chloride and being obtained as ruthenium(III) chloride solution; c) if appropriate, the ruthenium(III) chloride solution from step b) is worked up further.

    摘要翻译: 本发明涉及一种用于从使用的含钌催化剂中回收钌的方法,其中将钌作为氧化钌在微溶于无机酸的载体材料上包括以下步骤:a)将包含氧化钌的催化剂在 存在于载体上的氧化钌还原成金属钌; b)在载体材料上包含金属钌的步骤a)的还原催化剂在含氧气体存在下用盐酸处理,载体上存在的金属钌以氯化钌(III)的形式溶解并得到 作为氯化钌(III)溶液; c)如果合适,将步骤b)的氯化钌(III)溶液进一步处理。