WO2010040468A2 - Catalyseur à base d'uranium et son procédé de fabrication ainsi que son utilisation - Google Patents

Catalyseur à base d'uranium et son procédé de fabrication ainsi que son utilisation Download PDF

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Publication number
WO2010040468A2
WO2010040468A2 PCT/EP2009/007039 EP2009007039W WO2010040468A2 WO 2010040468 A2 WO2010040468 A2 WO 2010040468A2 EP 2009007039 W EP2009007039 W EP 2009007039W WO 2010040468 A2 WO2010040468 A2 WO 2010040468A2
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WO
WIPO (PCT)
Prior art keywords
catalyst
uranium
alkaline earth
alkali
chlorine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2009/007039
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German (de)
English (en)
Other versions
WO2010040468A3 (fr
Inventor
Aurel Wolf
Leslaw Mleczko
Oliver Felix-Karl SCHLÜTER
Stephan Schubert
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Bayer AG
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Bayer Technology Services GmbH
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Publication date
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Publication of WO2010040468A2 publication Critical patent/WO2010040468A2/fr
Publication of WO2010040468A3 publication Critical patent/WO2010040468A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/12—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of actinides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/031—Precipitation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B7/00—Halogens; Halogen acids
    • C01B7/01—Chlorine; Hydrogen chloride
    • C01B7/03—Preparation from chlorides
    • C01B7/04—Preparation of chlorine from hydrogen chloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2235/00—Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties
    • B01J2235/15—X-ray diffraction

Definitions

  • the present invention relates to a novel uranium catalyst, to a process for its preparation by precipitation from a solution and to its use in the course of processes for the production of chlorine from hydrogen chloride. Almost all of the technical production of chlorine today takes place through the electrolysis of aqueous saline solutions.
  • catalysts comprising transition metals and / or noble metals for the conversion of hydrogen chloride to chlorine.
  • catalysts comprising at least one of copper, potassium, sodium, chromium, cerium, gold, bismuth, ruthenium, rhodium, platinum and the elements of VQI. Subgroup of the Periodic Table of the Elements can be used for this purpose. It is further disclosed that the oxides, halides or mixed oxides / halides of the aforementioned elements are preferably used. Particular preference is given to copper chloride, copper oxide, potassium chloride, sodium chloride, chromium oxide, bismuth oxide, ruthenium oxide, ruthenium chloride, ruthenium oxychloride and also rhodium oxide.
  • WO 2007 134771 these catalysts are distinguished by a particularly high activity for the conversion of hydrogen chloride to chlorine.
  • WO 2004 052776 discloses that it is a well-known problem in the field of heterogeneous catalytic oxidation of hydrogen chloride to chlorine that so-called "hot spots" are formed in the processes These hot spots designate places of a disproportionate one Temperature increase, which according to the disclosure of WO 2004 052776 can lead to the destruction of the catalyst material.
  • WO 2004 052776 discloses as a solution to this technical problem, the execution of a cooled process in tube bundles.
  • the technical solution disclosed in WO 2004 052776 comprises the cooling of the contact tubes.
  • the alternative technical solution disclosed in WO 2007 134771 comprises the multistage adiabatic exports of the process with interstage cooling.
  • EP 1 170 250 A further alternative to the complicated apparatus of solving the above-mentioned problems with respect to the catalysts is disclosed in EP 1 170 250.
  • the excessively high temperatures in the region of the reaction zones are counteracted by reduced catalyst beds with reduced reaction times Activity of the catalyst can be used.
  • Such adapted catalyst beds are achieved, for example, by "diluting" the catalyst beds with inert material, or simply by providing reaction zones with a lower proportion of catalyst, but the process disclosed in EP 1 170 250 is disadvantageous because such "dilution" reaction zones with a desired low space-time yield can be created.
  • the catalysts disclosed in DE 1 078 100 include support materials such as kaolin, silica gel, kieselguhr, pumice, etc.
  • the catalysts are prepared by applying the uranium from the solution to the support. It is not disclosed that the catalysts can be obtained by precipitation. Further, the disclosed catalysts do not comprise uraniumates comprising sodium and uranium.
  • the maximum achievable conversion which can be achieved in DE 1 078 100 with the catalysts is 62%, which is small and thus disadvantageous in comparison with the conversions possible according to the disclosures set out above. This is especially true since 600 cm 3 of the reactor are filled with the catalyst in the specific embodiment in which said 62% conversion is achieved. This in turn means that in the further information, the activity of the catalyst seems to be quite low.
  • uranium oxide catalysts which consist in a preferred development only of uranium oxide, or which consist in the general case of a support of uranium oxide and another catalytic component.
  • Such further catalytically active components may be substances already disclosed in WO 2007 134771, for example.
  • the catalysts comprising the support of uranium oxide and a further catalytically active component can be obtained according to PCT / EP2008 / 005183 by impregnating the further catalytically active component on the support of uranium oxide.
  • the catalysts may comprise promoters, wherein these alkali, alkaline earth and rare earth metals may be especially sodium, cesium, strontium, barium and / or cerium.
  • these promoters are subsequently applied to the catalyst.
  • the catalysts disclosed in PCT / EP2008 / 005183 are disclosed as being particularly stable, so that they are advantageous over the catalysts used according to the disclosures of WO 2004 052776, WO 2007 134771 and EP 1 170 250.
  • the catalysts have quite high productivity at temperatures of 540 0 C and 600 0 C according to the embodiments of PCT / EP2008 / 005183.
  • a catalyst for the heterogeneous catalytic oxidation of hydrogen chloride to chlorine characterized in that the catalyst comprises a uranate of at least one alkali and / or alkaline earth metal, can achieve this object.
  • Uranates in the context of the present invention refer to materials containing uranium and oxygen in any stoichiometric or non-stoichiometric composition having negative charges.
  • Uranates are preferably negatively charged substances having a composition of UO ⁇ , where X is a real number greater than 1 but less than or equal to 5.
  • the at least one alkali and / or alkaline earth metal contained in the catalyst according to the invention denotes any substance of the first or second main group of the Periodic Table of the Elements.
  • Preferred alkali and / or alkaline earth metals are those selected from the list containing barium, calcium, cesium, potassium, lithium, magnesium, sodium, rubidium and strontium.
  • Particularly preferred are those selected from the list containing barium, calcium, potassium, magnesium and sodium.
  • q represents the number of positive charges that the alkali or alkaline earth metal has.
  • Preferred uraniumates of alkali or alkaline earth metals are Na 6 U 7 Oa 4 or Ba 3 U 7 O 24. The sodiumuranate Na 6 U 7 O 24 is particularly preferred.
  • the catalysts according to the invention have the same preferred and high stabilities as already disclosed in PCT / EP2008 / 005183, but at the same time have a drastically increased activity for the heterogeneous catalytic oxidation of hydrogen chloride to chlorine ,
  • the catalyst according to the invention may also comprise further substances in addition to the uranate of at least one alkali and / or alkaline earth metal.
  • the catalyst in addition to the uranate of at least one alkali and / or alkaline earth metal, also comprises uranium oxide.
  • Uranium oxide in the context of the present invention refers to stoichiometric and nonstoichiometric substances containing uranium and oxygen. Examples of stoichiometric substances are about UO 3 , UO 2 and UO. Possible non-stoichiometric substances resulting from mixtures of these species in the sense of this invention are, for example, U 3 O 5 , U 2 O 5 , U 3 O 7 , U 3 O 8 , U 4 O 9 and Ui 3 O 34 .
  • Preferred uranium oxides have a general composition of more than UO 2 to U ⁇ 2.9 , these uranium oxides are understood according to the general formula UO ⁇ with 2 ⁇ X ⁇ 2.9 as uranium oxides or mixtures thereof and X indicates only the stoichiometric ratio between uranium and oxygen in the compound.
  • the catalyst in addition to the uranium of at least one alkali and / or alkaline earth metal also salts and / or oxides of alkali and / or alkaline earth metals.
  • Another object of the present invention is a process for the preparation of the inventive catalysts, characterized in that a) a uranium salt is precipitated by adding a strong alkali and / or alkaline earth liquor from a homogeneous, aqueous solution containing a precipitate A, and b) the Precipitate A is subsequently separated from the aqueous solution and dried.
  • Uranium salt in the context of the present invention means any compound comprising at least one ion of the element uranium with at least one counter-ion, wherein the total of optionally a plurality of counter-ions in total carries as many opposite charges as the totality of the optionally contained more uranium ions ,
  • the uranium ions in the uranium salt according to the invention may be charged twice, three times, four times, five times or six times positively.
  • the uranium ions in the uranium salt are four, five or six times positively charged.
  • the uranium ions of the uranium salt are six times positively charged.
  • Preferred uranium salts are uranyl oxide acetate UO 2 Ac 2 and uranium oxide nitrate UO 2 (NO 3 ) 2 .
  • uranium salts are particularly advantageous because they can be dissolved in aqueous solutions in high proportions and at the same time the acetate and nitrate radicals with the alkali and / or alkaline earth metal ions of the alkali and / or alkaline earth liquors are completely dissociated in water, so they are not together with the precipitate A precipitate and contaminate the precipitate.
  • these uranium salts are particularly advantageous because they are reacted in drying at step b), at the preferred temperatures in gaseous nitrogen oxides or gaseous carbon oxides, such as carbon monoxide or carbon dioxide and thus can no longer contaminate the catalyst obtained.
  • Strong alkali and / or alkaline earth liquors in the context of the present invention designate lyes comprising at least one ion of an alkali and / or alkaline earth metal.
  • Preferred strong alkali and / or alkaline earth liquors are those having a pKa of 9.25 or greater. Preference is given to bases having a pKa value of 15 or more.
  • Particularly preferred alkali and / or alkaline-earth liquors are sodium hydroxide, potassium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide and / or sodium aluminates, such as NaAl (OH) 4 .
  • the homogeneous aqueous solution present in the process according to step a) denotes solutions in which all substances are present in molecular solution.
  • the aqueous solution of step a) before addition of the strong liquor has a pH which is less than or equal to 7.
  • the person skilled in the art will have suitable means for achieving this.
  • precursors of the advantageous catalysts according to the invention comprising a uranate of at least one alkali and / or alkaline earth metal are obtained in step a) by mixing the precipitate A at this time as a mixed form between uranium oxide, uranium hydroxide, alkali and / or alkaline earth lanthanate, alkali metal and / or alkaline earth metal hydroxide and / or one of the hydrates of the aforementioned, is present in the aqueous solution as a solid.
  • the proportions of the alkali metal and / or alkaline earth metal hydroxides in this mixed form result from the fact that precipitation from the solution entrains them at least partially and thus includes them in the precipitate A. As a result, it may also happen that uranium oxide and / or uranium hydroxide is included in the precipitate, which has not been rearranged with the alkali and / or alkaline earth metal ions to the uranium.
  • step a) is carried out so that the strong alkali and / or alkaline earth liquor is simultaneously supplied with a homogeneous aqueous solution of a uranium salt in a container so that the uranium salt is precipitated from this solution as precipitate A.
  • the precipitation according to the inventive step a) as well as according to the step a) according to the preferred embodiment of the method can be carried out continuously or discontinuously.
  • step a) of the process can be carried out in devices generally known to those skilled in the art for achieving a high mixing intensity between the homogeneous aqueous solution of a uranium salt and the strong alkali and / or alkaline earth liquor.
  • An overview of advantageous devices and modes of operation, in particular for continuous methods for precipitation, is given for example by WO 2007 093337.
  • Preferred devices in which such failure is carried out are nozzles and / or micromixers.
  • the preferred devices are particularly advantageous because they can be integrated in an advantageous manner in continuous processes for the preparation of the catalysts of the invention.
  • the precipitation can also be carried out in stirred containers.
  • the precipitate A is separated from the water and by drying the optionally still present mixed form between uranium oxide, uranium hydroxide, alkali and / or alkaline earth metal, alkali and / or alkaline earth metal hydroxide and / or one of the hydrates of the aforementioned in the uraniumate according to the invention is converted at least one alkali and / or alkaline earth metal, or optionally further converted uranium hydroxides and / or Uranoxidhydrate converted into uranium oxide.
  • Step b) of the method according to the invention can be carried out according to embodiments generally known to the person skilled in the art.
  • the separation of water according to step b) of the process according to the invention can be carried out, for example, by centrifugation, filtration, freeze-drying or other generally known processes using devices likewise generally known to the person skilled in the art.
  • step b) of the process according to the invention can be carried out under atmospheric pressure (1013 hPa) or under reduced atmospheric pressure, it being preferred to carry out drying under reduced pressure to atmospheric pressure.
  • the drying can be carried out at room temperature (23 ° C.) or at a temperature which is elevated relative to room temperature, it being preferred to carry out the drying at a temperature which is higher than room temperature. It is particularly preferred to carry out the drying at temperatures of 500 ° C. to 1500 ° C.
  • the drying can also be carried out in several stages in alternative embodiments of step b) of the process according to the invention. Preference is given in such alternative embodiments predrying at room temperature to 250 0 C and a subsequent drying at temperatures of 500 0 C to 1500 0 C. Such temperatures of 500 0 C to 1500 0 C are particularly advantageous because this certainly all possibly still in Preciproduct A contained hydroxides and hydrates are thus converted to oxides and / or salts, and thus the erf ⁇ ndungswashen uranium of at least one alkali and / or alkaline earth metal are preferably formed.
  • the erf ⁇ ndungssiee drying or post-drying according to the alternative embodiment of the erf ⁇ ndungssieen method at 500 0 C to 1500 0 C may in this respect also under the well-known to those skilled in the term of "calcining" summarized.
  • washing of the precipitate A is provided between step a) and step b) of the process.
  • This washing is preferably carried out with water.
  • Such a washing is advantageous because it allows residues of alkali and / or alkaline earth liquor or uranium salt, which may have been deposited on the surface of the precipitated product A, to be washed off, so that the catalysts obtained after step b) of the process according to the invention are present on the surface have the desired composition.
  • Another object of the present invention are processes for the preparation of chlorine, characterized in that in a reaction zone hydrogen chloride in the presence of uranium of at least one alkali and / or alkaline earth metal is oxidized to chlorine.
  • Such processes are preferably operated at temperatures above 400 0 C in a reaction zone. Operation at such temperatures is particularly advantageous because the uranates of at least one alkali and / or alkaline earth metal are particularly active, but at the same time stable, especially at these temperatures.
  • the catalysts according to the invention which are preferably prepared by the process presented here, are preferably used in the abovementioned processes for preparing chlorine, since it has surprisingly been found that they are temperature-stable but at the same time substantially more active than catalysts for the abovementioned oxidation of hydrogen chloride to chlorine, as comparably stable catalysts.
  • Another object of the present invention is therefore the use of uraniumates of at least one alkali and / or alkaline earth metal as a catalyst for the oxidation of hydrogen chloride to chlorine.
  • FIG. 1 An embodiment of a preferred variant of this invention is shown in Fig. 1, without the invention being limited thereto. Not erf ⁇ ndungswashe variants are shown in Figs. 2 to 3.
  • Fig. 1 shows a powder X-ray diffractogram a) of a catalyst according to the invention comprising Na 6 U 7 O 2 ⁇ prepared according to Example 1, and hereunder idealized spectra used to identify the phases U 3 O 8 b), as well as Na 6 U 7 O 24 c) according to Example 1 were used.
  • the intensity of the X-ray signal (I) is shown in each case over the angle 2 ⁇ .
  • Fig. 2 shows a powder X-ray diffractogram a) of a catalyst not according to the invention, which was prepared according to the Comparative Example 1, and below an idealized spectrum, which was used to identify the phase U 3 O 8 b). Shown is the intensity of the X-ray signal (I) over the angle 2 ⁇ .
  • FIG. 3 shows a powder X-ray diffractogram a) of a further catalyst not according to the invention, which was prepared according to the counter-example 2, and below an idealized spectrum which was used for the identification of the phase U 3 Og b). Shown again is the intensity of the X-ray signal (I) over the angle 2 ⁇ .
  • Example 1 Preparation of a catalyst according to the invention
  • the contents of the beaker and further beaker were then added via dropping funnel into the three-necked flask by adding dropwise.
  • the contents of the other beaker were added so that a pH of 10.5, measured by the pH measuring device, was maintained constant.
  • a cloudy precipitate formed in the three-necked flask.
  • the resulting solid was filtered through a suction filter and washed with distilled water until the washings were neutral (pH ⁇ 7). Subsequently, the solid was predried under air and ambient pressure for 2 h at 90 0 C and subsequently dried at 800 0 C for 4 h.
  • Example 2 (comparative example): Preparation of a first catalyst not according to the invention by pyrolysis
  • Example 3 (comparative example): forming a further catalyst not according to the invention 2 g of powdered uranium (V / VI) oxide (from Strem Chemicals.) Were pre-dried overnight at 150 0 C in a drying oven at ambient pressure and then for 2 h in air at 800 0 C treated. The powder was investigated analogously to Example 1 powder X-ray diffractometry, with only one was identified (see Fig. 3).
  • Examples 4-6 Use of the Catalysts of Examples 1-3 for the Heterogeneous Catalytic Oxidation of Hydrogen Chloride to Chlorine at 400 ° C.
  • 0.2 g of the substances obtained according to Examples 1 to 3 were ground by hand in a mortar and mixed with 1 quartz sand (100-200 ⁇ m) was introduced into a quartz reaction tube (diameter ⁇ 10 mm).
  • the quartz reaction tube was heated to 400 0 C and operated in the following at this temperature.
  • a gas mixture of 80 ml / min of hydrogen chloride and 80 ml / min of oxygen was passed through the quartz reaction tube.
  • the product gas stream was passed into a 16% by weight potassium iodide solution for 10 minutes and the resulting iodine was back titrated with a 0.1 N thiosulfate solution to determine the amount of chlorine introduced. From this, the activities shown in Table 1 of the substances according to Examples 1 to 3 at 400 0 C were calculated.
  • Examples 7-9 Use of the catalysts of Examples 1-3 for the heterogeneous catalytic oxidation of hydrogen chloride to chlorine at 500 0 C Experiments were analogous to those of Examples 4-6 performed, where the only difference is now the quartz reaction tube to 500 0 C was heated and subsequently operated at this temperature.
  • Examples 10-12 Use of the catalysts from Examples 1-3 for the heterogeneous catalytic oxidation of hydrogen chloride to chlorine at 540 ° C.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un nouveau catalyseur à base d'uranium, son procédé de fabrication par précipitation à partir d'une solution ainsi que son utilisation dans le cadre de procédés de production de chlore à partir de chlorure d'hydrogène.
PCT/EP2009/007039 2008-10-09 2009-10-01 Catalyseur à base d'uranium et son procédé de fabrication ainsi que son utilisation Ceased WO2010040468A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008050978.7 2008-10-09
DE102008050978A DE102008050978A1 (de) 2008-10-09 2008-10-09 Urankatalysator und Verfahren zu dessen Herstellung sowie dessen Verwendung

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WO2010040468A2 true WO2010040468A2 (fr) 2010-04-15
WO2010040468A3 WO2010040468A3 (fr) 2010-07-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106749357A (zh) * 2016-12-01 2017-05-31 辽宁师范大学 二维金属铀氧簇配合物及其合成方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009013905A1 (de) 2009-03-19 2010-09-23 Bayer Technology Services Gmbh Urankatalysator auf Träger besonderer Porengrößenverteilung und Verfahren zu dessen Herstellung, sowie dessen Verwendung

Family Cites Families (9)

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Publication number Priority date Publication date Assignee Title
DE1078100B (de) 1958-12-23 1960-03-24 Wolfen Filmfab Veb Katalysatoren fuer die katalytische Oxydation von Chlorwasserstoff
DE1195726B (de) * 1960-01-20 1965-07-01 Shell Int Research Katalysator zur Herstellung von Chlor
EP0170250B1 (fr) 1984-07-31 1990-10-24 Kabushiki Kaisha Toshiba Transistor bipolaire et son procédé de fabrication
US4677091A (en) * 1985-07-15 1987-06-30 The Standard Oil Company Process for the preparation of mixed metal oxide catalysts
US6977066B1 (en) 1999-01-22 2005-12-20 Sumitomo Chemical Company, Limited Method for producing chlorine
DE10258153A1 (de) 2002-12-12 2004-06-24 Basf Ag Verfahren zur Herstellung von Chlor durch Gasphasenoxidation von Chlorwasserstoff
DE102006007147A1 (de) 2006-02-16 2007-08-23 Bayer Technology Services Gmbh Verfahren zur kontinuierlichen Herstellung von Katalysatoren
DE102007020140A1 (de) * 2006-05-23 2007-11-29 Bayer Materialscience Ag Verfahren zur Herstellung von Chlor durch Gasphasenoxidation
WO2009010167A1 (fr) 2007-07-13 2009-01-22 Bayer Technology Services Gmbh Catalyseur thermiquement stable pour l'oxydation de chlorure d'hydrogène en phase gazeuse

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106749357A (zh) * 2016-12-01 2017-05-31 辽宁师范大学 二维金属铀氧簇配合物及其合成方法

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WO2010040468A3 (fr) 2010-07-22

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