Supported metals incipient wetness

Catalysts are prepared by impregnation by spraying a solution of a metal salt onto pellets of a porous support until incipient wetness. The pellets are then dried and calcined to transform the metal into insoluble form. 

Impregnation of Supports and Drying. Most obvious is incipient wetness impregnation of a support with a solution of an active precursor and subsequent drying and calcination of the thus loaded support [6], Incipient wetness or pore-volume impregnation is especially attractive with preshaped support bodies. When the active component has to be in the metallic state, reduction can be carried out after the calcination step. Often, the catalyst is reduced after loading into the reactor to prevent a separate passivation step, in which the surface of the pyrophoric reduced catalyst is carefully oxidized. However, to achieve reproducible catalysts the catalyst manufacturer usually reduces the catalyst and delivers the passivated catalyst, which then only needs a short additional reduction. 

Palladium was deposited onto three different supports by incipient-wetness impregnation, as described elsewhere [16]. The supports, supplied by Condea GmbH, possess the following chemical composition AI2O3, Ba-Al203 and La-ALOs. The concentration of Ba and La, respectively, was 3 wt% for both supports. A Pd(N03)2 solution (Alfa Aesar, 8.41 wt%) was used as the metal precursor. The concentration of the solution was calculated to obtain a washcoat with a metal loading of 2.5 wt %. 

A 5 wt.% CoOx/Ti02 catalyst was prepared via an incipient wetness technique in which an aqueous solution of Co(N03)2 6H20 (Aldrich, 99.999%) was impregnated onto a shaped Ti02 (Milleimium Chemicals, commercially designated as DT51D, 30/40 mesh), as described in detail elsewhere [6]. Other supported metal oxide catalysts, such as FeOx, CuO, and NiOx, were obtained in a fashion similar to that used for preparing the CoO, catalyst. 

Catalysts were prepared on various supports. One example was a Calgon 120% CTC coconut carbon. The impregnation volume of metal solution was calculated using the measured incipient wetness of the support 0.85 cc liquid per gram of carbon for the... 

Catalysts - A commercial Raney nickel (RNi-C) and a laboratory Raney nickel (RNi-L) were used in this study. RNi-C was supplied in an aqueous suspension (pH < 10.5, A1 < 7 wt %, particle size 0.012-0.128 mm). Prior to the activity test, RNi-C catalyst (2 g wet, 1.4 g dry, aqueous suspension) was washed three times with ethanol (20 ml) and twice with cyclohexane (CH) (20 mL) in order to remove water from the catalyst. RCN was then exchanged for the cyclohexane and the catalyst sample was introduced into the reactor as a suspension in the substrate. RNi-L catalyst was prepared from a 50 % Ni-50 % A1 alloy (0.045-0.1 mm in size) by treatment with NaOH which dissolved most of the Al. This catalyst was stored in passivated and dried form. Prior to the activity test, the catalyst (0.3 g) was treated in H2 at 250 °C for 2 h and then introduced to the reactor under CH. Raney cobalt (RCo), a commercial product, was treated likewise. Alumina supported Ru, Rh, Pd and Pt catalysts (powder) containing 5 wt. % of metal were purchased from Engelhard in reduced form. Prior to the activity test, catalyst (1.5 g) was treated in H2 at 250 °C for 2 h and then introduced to the reactor under solvent. 10 % Ni and 10 % Co/y-Al203 (200 m2/g) catalysts were prepared by incipient wetness impregnation using nitrate precursors. After drying the samples were calcined and reduced at 500 °C for 2 h and were then introduced to the reactor under CH. 

Catalysts were prepared by incipient wetness impregnation of commercial supports using cobalt nitrate as a precursor. Metallic cobalt species were active centers in the ethanol steam reforming. Over 90% EtOH conversion achieved. Nature of support influences the type of byproduct formation. Ethylene, methane and CO are formed over Co supported on A1203, Si02 and MgO, respectively... 

In this series of experiments, the catalysts were used over five repeat contacts with fresh coal liquid. Point of Ayr coal liquid was supplied by the British Coal Corporation, Coal Research Establishment (CF ) one batch of this coal liquid was used in experiments with CoMo and NiMo catalysts and a further batch was used in experiments with ZnMo and ZnW. The catalysts were prepared as extrudates by the technique of incipient wetness which requires stirring the dry alumina support with a set volume of a pre-determined concentration of an appropriate soluble salt of the metal such that the pore space is just taken up by the metals at the required concentration. The alumina support was supplied by Akzo Chemie, The Netherlands and the catalysts were made up to contain 15% WO3 or M0O3 and 3% NiO, CoO, or ZnO, expressed as a weight percentage of the weight of support... 

Several methods were used to incorporate Pt metal onto the magnesia support. One method involved the impregnation of aqueous H2PtCl6 onto the dried support until the point of incipient wetness. A second method utilized vapor phase... 

In impregnation the pores of the support are filled with a solution of the gold precursor. Where just the needful volume is used, the method is impregnation to incipient wetness, but sometimes an excess of solution is used and the solvent removed by evaporation, so that concentrated solution finally resides in the pores (Sections 4.2.1 and 4.3.1). In these methods, the metal dispersion ultimately obtained depends critically on the conditions of drying.1... 

We will try to separate as far as possible the procedures of preparation from the chemical reactions that occur during these preparations. For instance in the case of impregnation to incipient wetness, both the metal ions and the counter-ions are deposited on the support, but the speciation of the metal-containing ions may vary with the pH of the solution in contact with the support, and the way in which they interact with the support will also depend on the PZC of the support. 

---