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  • B01J29/405—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively containing rare earth elements, titanium, zirconium, hafnium, zinc, cadmium, mercury, gallium, indium, thallium, tin or lead
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Definitions

• MTG methanol-to-gasoline
• MTO methanol-to-olefins
• MTP methanol-to-propylene
• a catalyst may be optimized to emphasize various functions such as product yield or selectivity. However, when one function is optimized the resulting catalyst will often show less advantageous with respect to other parameters.
• An example may be a catalyst optimized to achieve a higher product yield but which then shows a decreased selectivity. Thus, a special task in developing new catalyst is to improve the catalyst on essential parameters without adverse effect to other important features.
• a catalyst which enables an improved aromatics yield
• a catalyst which enables a reduced MeOH cracking to non-desired products such as CO and CO 2 .
• a catalyst which substantially regains activity after regeneration.
• a bifunctional catalyst for example for conversion of oxygenates and dehydrogenation of hydrocarbons, said catalyst comprising zeolite, alumina binder and Zn, wherein the Zn is present at least partly as ZnAl 2 O 4 .
• a bifunctional catalyst containing acidic zeolite sites as well as dehydrogenation sites e.g. metal or oxide is provided.
• the catalyst is optimized for conversion of oxygenates such as methanol and/or DME into aromatics (herein abbreviated MTA).
• the binder may be a pure alumina binder or an alumina-based binder further comprising mixtures of aluminum oxide and aluminum hydroxide and/or e.g. silica/alumina.
• the zeolite may for example be one of the commonly known zeolites used in MTA and MTG processes.
• H-ZSM-5 may be a preferred zeolite for the present catalyst due to its unique pore structure leading to favorable size selectivity as well as its relatively low coking rate. H-ZSM-5 may be particularly preferred in case of MTA processes.
• Zn/ZSM-5 catalysts with low content of Zn such as 1 wt % Zn for MTA are known and it has been argued that higher Zn content is to be avoided in order to avoid methanol cracking to carbon oxides.
• the applicant has shown that a high Zn content in the catalyst may result in an improved aromatics yield in MTA processes compared to known catalysts.
• the total Zn content in the catalyst is 3-25 wt %, 5-20 wt %, 7-15 wt % or 8-13 wt %, such as more than 7 wt % Zn, more than 10 wt % Zn or 12 wt % or more Zn.
• the Zn in the catalyst may be present in various concentrations in both binder and zeolite of the present catalyst.
• the Zn concentration is higher in the binder phase than in the zeolite phase which for example may be the case where the Zn is applied by impregnation.
• a catalyst wherein Zn is present in both zeolite and alumina binder allows for industrial production by “simple” means such as by impregnation.
• a bifunctional catalyst as herein described may be achieved by Zn impregnation of a “base catalyst” comprising an alumina binder and a zeolite such as ZSM-5.
• a preferred base catalyst comprises 30-50% binder and 50-70% zeolite.
• the impregnation may be carried out by contacting the zeolite or the zeolite and alumina binder with a Zn-containing solution.
• the solution may preferably be aqueous, but other solvents than water may be preferred as well.
• Impregnation may also be carried out by contacting the zeolite or the zeolite and alumina binder with a solid Zn compound, e.g., by mixing and/or grinding or other treatments to ensure intimate mixing of the components.
• the Zn source may be any Zn-containing, organic and/or inorganic, compound.
• Preferred compounds comprise zinc nitrate, zinc acetate and zinc oxide, hydroxide, carbonate or mixtures hereof.
• impregnation will typically be followed by calcination or similar treatment(s).
• zeolite or an alumina/zeolite based catalyst is impregnated with Zn in order to obtain the desired amount of Zn in the zeolite
• significant amounts of Zn may also be introduced into the binder, for example, as ZnO and/or ZnAl 2 O 4 .
• Various ratios of ZnO/ZnAl 2 O 4 may be achieved depending on the treatment of the impregnated catalyst.
• Zn in the alumina binder is present mainly as ZnAl 2 O 4 .
• the Zn in the binder has been fully spinelized, according to the reaction equation ZnO+Al 2 O 3 ⁇ ZnAl 2 O 4 , meaning that all or substantially all of the Zn in the binder is present as ZnAl 2 O 4 .
• a large part of the Zn in the alumina binder is present as ZnAl 2 O 4 .
• Defining the relative amount of ZnAl 2 O 4 in the binder phase as molar percentage of Zn present as ZnAl 2 O 4 relative to the total amount of Zn contained in the binder phase in some embodiments 50-100% of the Zn in the binder is present as ZnAl 2 O 4 , for example more than 60%, more than 70% or more than 80%. In some advantageous embodiments 85-100% of the Zn in the binder is present as ZnAl 2 O 4 , such as more than 90% or more than 95%.
• ZnAl 2 O 4 As shown by the applicant cracking of MeOH may be avoided with a high degree of spinelization, it may be preferred especially in case of high Zn content in the catalyst that more than 97% of the Zn in the binder is present as ZnAl 2 O 4 , such as more than 98%, more than 99%, more than 99.5% or more than 99.8% of the Zn in the binder is present as ZnAl 2 O 4 .
• Optimal and practically achievable ZnAl 2 O 4 content ranges may be 95-100% in the binder is present as ZnAl 2 O 4 , such as 97%-99.9% Zn in the binder is present as ZnAl 2 O 4 .
• the catalyst has been fully spinelized meaning that all or substantially all of the Zn in the binder is present as ZnAl 2 O 4 .
• ZnO in the binder is active in cracking methanol which is an undesired reaction in MTA.
• more or less of the Zn in the alumina binder may be present as ZnAl 2 O 4 .
• Steaming or calcination of a Zn impregnated catalyst as commonly applied in production of metal/zeolite systems may result in a partial spinelization of the Zn (ZnO+Al 2 O 3 ->ZnAl 2 O 4 ).
• the fresh (start of run) catalyst has a CO x selectivity (determined at 420° C., 20 bar, 10 mol % methanol and a WHSV of 1.6) below 8% preferably below 7% such as 6% or below, or 5% or lower, or even 2% or lower.
• the CO x selectivity is defined as the molar percentage of methanol in the feed converted into CO and CO 2 according to the net reactions:
• a preferred bifunctional catalyst comprising alumina binder, H-ZSM-5 and 8-15 wt % Zn in the total catalyst and where the Zn in the binder is fully or substantially fully spinelized.
• Said catalyst provides a high aromatics yield in a MTA reaction while cracking of the methanol is reduced to below 7%.
• An exemplary bifunctional catalyst may desirably comprise 30-65 wt % H-ZSM-5, 5-40 wt % ZnAl 2 O 4 , 0-40 wt % Al 2 O 3 , 0-10 wt % ZnO.
• the catalyst may further in some embodiments be characterized by having 0.1-12 wt % such as 1-7 wt % Zn present in the zeolite phase.
• it may comprise 50-60 wt % H-ZSM-5, 10-35 wt % ZnAl 2 O 4 , 2-25 wt % Al 2 O 3 , 0-7 wt % ZnO.
• it may be beneficial to have at least a small excess of Al 2 O 3 which is not spinelized in reaction with ZnO. Using a higher amount of Al 2 O 3 in the preparation of the “base catalyst” will lead to a more robust catalyst preparation process.
• a partially spinelized catalyst with a moderate to high ZnAl 2 O 4 :ZnO ratio may e.g. be obtained by heating the Zn-impregnated base catalyst at 300-500° C. in air.
• a partially spinelized catalyst with a very high ZnAl 2 O 4 :ZnO content, fully spinelized catalyst or a substantially fully spinelized catalyst may be obtained by heating the Zn impregnated catalyst at 300-550° C. in steam or in an atmosphere comprising at least 10 vol %, 30 vol % 50 vol % or 80 vol % steam.
• a partially spinelized catalyst with a very high ZnAl 2 O 4 :ZnO content, fully spinelized catalyst or a substantially fully spinelized catalyst may be obtained by heating a partially spinelized catalyst at 300-550° C. in steam or in an atmosphere comprising at least 10 vol %, 30 vol % 50 vol % or 80 vol % steam.
• An at least partially spinelized catalyst preferably a partially spinelized catalyst with a very high ZnAl 2 O 4 content, fully spinelized catalyst or a substantially fully spinelized catalyst as described herein may be provided in numerous ways including obtaining a desired spinelized catalyst during production or by producing a catalyst with a spinelization degree below the desired spinelization percentage and followed by steaming said catalyst in a subsequent step e.g. as in an in situ steaming step to obtain a catalyst with a desired degree of spinelization.
• the two components may constitute an integrated entity, e.g. as obtained by introducing the Zn component by impregnation or ion-exchange to the zeolite, either onto the zeolite itself or onto an extrudate in which the zeolite is embedded in an alumina binder.
• the Zn component may also be added in the form of a salt, either as a solid or in solution, or an oxide, hydroxide or carbonate together with the zeolite, binder and/or lubricants prior to shaping, e.g. during extrusion or pelletization.
• the post-impregnation treatment (calcination or similar heat treatment) is preferably carried out in a humid atmosphere, e.g., by heating the Zn impregnated base catalyst at 300-550° C. in steam or in an atmosphere comprising at least 10 vol %, 30 vol % 50 vol % or 80 vol % steam.
• a method for producing a bifunctional catalyst comprising an alumina binder, zeolite and Zn, said method comprising the steps of
• a base catalyst containing 65 wt % H-ZSM-5 and 35% Al 2 O 3 was prepared by mixing followed by extrusion following well known procedures. Upon calcination, samples of the base catalyst were impregnated with an aqueous solution containing zinc nitrate at different Zn concentrations. The resulting pore-filled extrudates were heated to 470° C. in air and kept at 470° C. for 1 h to obtain catalysts with various amounts of Zn.
• Catalysts prepared by the procedure described in example 1 were subjected to conversion of methanol at 420° C. in an isothermal fixed bed reactor. N 2 was used as an inert co-feed to obtain a methanol concentration of 7 mol % in the reactor inlet. The total pressure was 20 bar, and the space velocity (WHSV) of methanol was 2 h ⁇ 1 .
• Zn/H-ZSM-5 catalysts suffer from reversible as well as irreversible deactivation.
• Deposition of carbon (coke) on the catalyst is responsible for reversible deactivation.
• the deactivated (coked) catalyst is regenerated by removal of the deposited carbon by combustion in a flow of 2% O 2 (in N 2 ) at 500° C.
• Wt % of aromatics in hydrocarbon product is defined as the mass of aromatics relative to the total mass of hydrocarbons in the effluent stream. Percentage of aromatics Aromatics in total hydro- selectivity regained after Zn content (wt %) carbon product (wt %) regeneration 5 52 90 10 51 95
• Wt % of aromatics in hydrocarbon product is defined as the mass of aromatics relative to the total mass of hydrocarbons in effluent stream.
• Cracking (decomposition) of methanol/DME can occur via several mechanisms.
• the acidic sites in the catalyst may catalyze cracking of DME to CH 4 , CO, and H 2 , while certain Zn species catalyze cracking of methanol to CO and H 2 .
• CO 2 can be formed as a primary cracking product or indirectly via the water gas shift reaction.
• Methanol conversion has been performed at 420° C., 20 bar, 10 mol % methanol (N2 balance), and a space velocity (WHSV) of 1.6.
• a base catalyst containing 65% ZSM-5 and 35% Al 2 O 3 was impregnated with aqueous zinc nitrate solution.
• the resulting pore filled extrudates were calcined in air and steam, respectively.
• the catalyst calcined in air was subjected to steaming after calcination. Methanol conversion over these catalysts was performed using the same conditions as in example 4.

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