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 1,4- butane-diol by combined gas-phase and liquid-phase hydrogenation
    6.
    发明申请
    Method for the production of 1,4- butane-diol by combined gas-phase and liquid-phase hydrogenation 失效
    通过组合气相和液相氢化生产1,4-丁二醇的方法

    公开(公告)号:US20050267318A1

    公开(公告)日:2005-12-01

    申请号:US10516923

    申请日:2003-06-10

    CPC分类号: C07C29/149 C07C31/207

    摘要: 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 7-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.

    摘要翻译: 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 主要含有烷基取代的7-丁内酯的产物; 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。

    Method for the production of 1,4- butanediol
    8.
    发明申请
    Method for the production of 1,4- butanediol 失效
    1,4-丁二醇生产方法

    公开(公告)号:US20050182281A1

    公开(公告)日:2005-08-18

    申请号:US10517263

    申请日:2003-06-10

    摘要: 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 10 to 100 bar into a first reactor or into a first reaction zone of a reactor and catalytically hydrogenating it in the gas phase to a product which contains mainly optionally alkyl-substituted y-butyrolactone; b) introducing the product stream obtained in this way into a second reactor or into a second reaction zone of a reactor at a temperature of from 140° C to 260° C. and catalytically hydrogenating it in the gas phase to optionally alkyl-substituted 1,4-butanediol; steps a) and b) being carried out at the same pressure; c) removing the desired product from intermediates, by-products and any unconverted reactants; d) optionally recycling unconverted intermediates into one or both hydrogenation stages, said hydrogenation stages each 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 an oxidic support, and the product mixture removed from the first hydrogenation stage being introduced without further purification into the second hydrogenation stage.

    摘要翻译: 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10-100巴的C 4-14二羧酸或其衍生物的气流引入第一反应器或第一反应 并将其在气相中催化氢化成主要包含烷基取代的γ-丁内酯的产物; b)将以这种方式获得的产物流引入第二反应器或反应器的第二反应区,温度为140℃至260℃,并将其在气相中催化氢化为任选烷基取代的1 ,4-丁二醇; 步骤a)和b)在相同的压力下进行; c)从中间体,副产物和任何未转化的反应物中除去所需的产物; d)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,所述氢化阶段各自使用包含<= 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%的氧化载体,并将从第一氢化步骤除去的产物混合物不经进一步纯化引入到 第二加氢阶段。

    Two-stage method for producing butane diol with intermediated separation of succinic anhydride
    10.
    发明申请
    Two-stage method for producing butane diol with intermediated separation of succinic anhydride 失效
    制备丁二酸酐中间分离丁二醇的两阶段方法

    公开(公告)号:US20060167323A1

    公开(公告)日:2006-07-27

    申请号:US10516922

    申请日:2003-06-11

    IPC分类号: C07C31/18

    CPC分类号: C07C29/149 C07C31/207

    摘要: 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 in the gas phase to a product which contains mainly optionally alkyl-substituted γ-butyrolactone; b) removing succinic anhydride from the product obtained in step a), preferably to a residual level of from

    摘要翻译: 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,并将其催化氢化为 气相至主要含有烷基取代的γ-丁内酯的产物; b)从步骤a)中获得的产物中除去琥珀酸酐,优选残留量为约0.3至0.2重量%; c)将步骤b)中获得的产物流在150℃至240℃的温度和15至100巴的压力下引入第二反应器,并将其在气相中催化氢化为任选的烷基 - 取代的1,4-丁二醇; d)从中间体,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步骤中,所述氢化步骤各自使用催化剂,所述催化剂包含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%的氧化载体,并且所述第二反应器具有比所述第一反应器更高的压力。