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:
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.
摘要:
The present invention provides a process for distillatively purifying crude water-containing tetrahydrofuran by passing the crude tetrahydrofuran through three distillation columns, withdrawing water from the bottom of the first column, recycling water-containing tetrahydrofuran from the top of the second column into the first column, passing a sidestream of the first column into the second column, recycling the bottom product of the third column into the first column, and withdrawing a distillate at the top of the first column, which comprises passing a sidestream of the second column into the third column and recovering the pure tetrahydrofuran as the top product of the third column.
摘要:
The present invention relates to a process for preparing unsubstituted or C1-C4-alkyl-substituted gamma-butyrolactone by catalytic hydrogenation of maleic acid and/or its derivatives in the presence of chromium-free catalyst comprising from 10 to 80% by weight of copper oxide and from 10 to 90% by weight of at least one catalyst support selected from the group consisting of silicon dioxide, titanium dioxide, hafnium dioxide, magnesium silicate, activated carbon, silicon carbide, zirconium dioxide and alpha-aluminum oxide.
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:
A process for coproducing alkyl-substituted or unsubstituted THF and pyrrolidones by catalytically hydrogenating C4-dicarboxylic acids and/or derivatives thereof in the gas phase in the presence of copper catalysts and reacting GBL with ammonia or primary amines to give pyrrolidones comprises a) hydrogenating C4-dicarboxylic acids and/or derivatives thereof in the gas phase at from 200 to 300° C., from 0.1 to 100 bar, catalyst hourly space velocities of from 0.01 to 1 kg of reactant/l of catalyst*hour and reactant/hydrogen molar ratios of from 20 to 800 in the presence of catalysts comprising copper, aluminum and/or zinc to give mixtures of THF and GBL, b) separating the hydrogenation effluent obtained by distillation into a THF/water mixture as the top product and a GBL-containing bottom product, c) separating the THF/water mixture from step b) in a distillation facility consisting of three columns by withdrawing water from the bottom of the first column, recycling water-containing THF from the second into the first column, passing a side stream of the first into the second column, recycling the bottom product of the third column into the first column and withdrawing a distillate at the top of the first column, wherein a side stream of the second column is passed into the third column and the pure THF is obtained as the top product of the third column, d) recovering GBL from the GBL-containing bottom product from step b) by distillation and e) reacting the GBL obtained with ammonia or amines to give corresponding pyrrolidones.
摘要:
The invention relates to a method of controlling a hydrogenation of a starting material in a hydrogenation reactor, in which the amount of hydrogen reacted in the hydrogenation is firstly determined, the ratio of the amount of hydrogen reacted to the amount of starting material fed in is then derived, this ratio is compared with a prescribed value and, finally, at least one process parameter is altered if the ratio of the amount of hydrogen reacted to the amount of starting material fed in deviates by a prescribed amount from the prescribed value.
摘要:
The present invention relates to a process for preparing optically active hydroxy-, alkoxy-, amino-, alkyl-, aryl- or chlorine-substituted alcohols or hydroxy carboxylic acids having from 3 to 25 carbon atoms or their acid derivatives or cyclization products by hydrogenating the correspondingly substituted optically active mono- or dicarboxylic acids or their acid derivatives in the presence of a catalyst whose active component consists of rhenium or of rhenium and comprises at least one further element having an atomic number of from 22 to 83, with the provisos that a. the at least one further element having an atomic number of from 22 to 83 is not ruthenium and b. in the case of the preparation of optically active 2-amino-, 2-chloro-, 2-hydroxy- and 2-alkoxy-1-alkanols by catalytically hydrogenating corresponding optically active 2-aminocarboxylic acids, 2-chlorocarboxylic acids, 2-hydroxycarboxylic acids and 2-alkoxycarboxylic acids or their acid derivatives, the at least one further element having an atomic number of from 22 to 83 is not palladium or platinum.
摘要:
A multi-zone jacketed pipe reactor (2; 60; 90; 130) for carrying out exothermic gaseous phase reactions and with at least one reaction zone (I) working with vaporisation cooling, at least one reaction zone (II) working with circulation cooling and, possibly, with additional zones (III, IV) is characterised in that one reaction zone (I) working with vaporisation cooling forms the first reaction zone to which is connected an additional reaction zone (II) working with circulation cooling. In this way there occurs at the beginning of the reaction, when the latter is most violent, very intensive cooling at a precisely controllable temperature and especially as well a temperature that is constant across the entire cross-section of the reactor while subsequently in a subsequent reaction zone working with circulating cooling by means of global counter-flow guidance of the heat transfer agent a constant cooling of the reaction gas is achieved.