Catalysts for producing paraxylene by methylation of benzene and/or toluene
A paraxylene and catalyst technology, applied in the field of catalysts for preparing paraxylene through the methylation of benzene and/or toluene, can solve the problems of short catalyst life/cycle, increased recovery cost, and reduced
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Embodiment 1
[0055] La-containing MCM-22 crystals were synthesized from a mixture prepared from the following components: 990 g of water, 80 g of hexamethylethyleneimine (HMI) (99% solution), 275 g of silicon dioxide, 74 g of sodium aluminate solution (45%) and 13.5 g of 50% sodium hydroxide solution and 15.2 g of lanthanum nitrate hexahydrate in 50 g of deionized water. The mixture has the molar composition shown in Table 1 below.
[0056] Table 1
[0057] SiO 2 / Al 2 o 3
～22.5 h 2 O / SiO 2
～14 Oh - / SiO 2
～0.15 Na + / SiO 2
～0.215 HMI / SiO 2
～0.19
[0058] The mixture was reacted for 72 hours at 320°F (160°C) in a 52 liter autoclave with stirring at 250 RPM. The product was filtered, washed with deionized water and dried at 250°F (121°C). The X-ray diffraction pattern of the as-synthesized material shows the typical pure phase of the MCM-22 topology. Scanning electron microscope (SEM) images of the as-synthesized mater...
Embodiment 2
[0061] The catalyst was prepared from a mixture of 80 parts (basis: calcined 538° C.) of La-MCM-22 crystals from Example 1 and 20 parts of Versal TM 300 pseudoboehmite (pseudoboehmite) alumina (basis: calcined 538 ° C). Add enough water to make an extrudable paste. A mixture of La-MCM-22 crystals, pseudo-boehmite alumina, and water was then extruded into an 80 / 20 1 / 20"Q extrudate, which was then dried at 121°C. Under nitrogen (N 2 ) at 538°C to decompose and remove the organic templating agent. Humidify the N with saturated air 2 The extrudate was calcined and exchanged with 1 N ammonium nitrate to remove sodium. After ammonium nitrate exchange, the extrudates were washed with deionized water to remove residual nitrate ions prior to drying. The ammonium exchanged extrudates were dried at 116°C and calcined at 534°C in air. The H-form extrudate has an alpha of 610, a hexane adsorption of 93.9 and a m of 518 2 / g surface area.
Embodiment 3
[0063] The unmodified MCM-49 catalyst was prepared from a mixture of 80 parts (basis: calcined at 538°C) of MCM-49 crystals and 20 parts of high surface area Versal TM 300 alumina (basis: calcined at 538°C). MCM-49, Versal TM A mixture of 300 alumina and water is extruded into 1 / 20" Quadra-lobe (Quadra-lobe), and then dried overnight at 121 ° C in a hot-pack oven. In nitrogen (N 2 ) at 538°C to decompose and remove the organic templating agent. Humidify the N with saturated air 2 The extrudate was calcined and exchanged with 1 N ammonium nitrate to remove sodium. After ammonium nitrate exchange, the extrudates were washed with deionized water to remove residual nitrate ions prior to drying. The ammonium exchanged extrudates were dried overnight at 121°C and calcined at 538°C in air. The extrudate of the H-form had an alpha of 520, a hexane adsorption of ~91, a total (micro+meso) surface area of 536 / (353+184), and a collidine ( collidine) adsorption.
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