Butanol catalytic reactor

Liquid propylene, gaseous carbon monoxide and hydrogen, and a soluble cobalt catalyst are fed to a high-pressure catalytic reactor. The reactor effluent goes to a flash tank, where all of the solution constituents are vaporized except the catalyst, which is recycled to the reactor. The reaction products are separated from unconsumed reactants in a multiple-unit process, and the product stream, which contains both butyraldehyde and /i-butanol, is subjected to additional hydrogenation with excess hydrogen, converting all of the butyraldehyde to butanol. 

Gupta and Douglas [AIChE J., 13 (883), 1967] have studied the catalytic hydration of isobutylene to f-butanol, using a cation exchange resin catalyst in a stirred tank reactor. 

For 2-butanol dehydrogenation, catalytic reactions were carried out at atmospheric pressure in a fixed bed flow-microreactor. The feed was 4.2 Nl/h of helium with a partial pressure of 8.5 kPa of 2-butanol. Reaction temperatures were from 373 K to 573 K. Concentrations of reactants and products were measured at the reactor outlet by on-line gas chromatography. 

IR spectra were recorded using a Specord 75-IR spectrometer. H and C NMR spectra were recorded on a MSL-400 Bruker spectrometer with TMS and butanol-1 as internal references. Catalytic tests were performed in a slurry reactor and a trickle flow column reactor in the presence of granulated (1.0-5-3,0 mm) and powdered 4.0%Pd/C catalysts. The reaction products were analyzed chromatographically (2 m x 3 mm column, [15% PEG-20M -i-2.5% KOH]/Chromaton-N). 

Their laboratory PVMR consisted of a reservoir in which the reactants were placed together with Nafion pellets, which acted as the catalyst. The liquid in the reservoir was continuously recirculated through the membrane tube, which was placed externally to the reactor. The membrane, itself, was also shown to be catalytic. A flow of inert gas (rather than vacuum) was used to remove the vapors and water from the membrane permeate. For the methanol esterification reaction the improvement in yield was modest (final conversion 77 % vs. 73 % corresponding to equilibrium), because the membrane was not very permselective towards the reaction products. Significant improvements, on the other hand, were observed with the butanol reaction (final conversion 95 % vs. 70 % corresponding to equilibrium), as the membrane is more permselective towards the products of this reaction. Exchanging the acidic protons in the Nafion membranes with cesium ions significantly improved the permselectivity, but also reduced membrane permeance. 

Catalytic tests with the lipase-monolithic catalysts were performed in a monolithic stirrer reactor consisting of a glass vessel equipped with a stirrer motor (V = 2.5 dm ). 1-Butanol and vinyl acetate concentrations were 0.6 M and 1 M, respectively. Activity tests with immobilized lipase Candida antarctica) were performed at varying stirrer rates and temperatures. Carbon monoliths (Westvaco integral carbon monoliths, with a loading of 30 wt% of microporous activated carbon, wall thickness 0.3 mm) were used as a reference material. 

By means of an ETHOS MR oven, Nuchter et al. [33] accomplished scaling-up of a microwave-assisted Fischer glycosylation to the kilogram scale with improved economic efficiency. In batch reactions, carbohydrates (o-glucose, o-mannose, d-galactose, butyl o-galactose, starch) were converted on the 50-g scale (95-100% yield, from 95 5 to 100%) with 3-30-fold molar excesses of an alcohol (methanol, ethanol, butanol, octanol) in the presence of a catalytic amount of acetyl chloride under pressure (microwave flow reactor, 120-140 °C, 12-16 bar, 5-12 min) or without applying pressure (120-140 °C or reflux temperature, 20-60 min). Furano-sides are not stable under these reaction conditions. 

The basis for this procedure for evaluating the concentration of absorbed species at reaction conditions rests upon being able to measure adsorption while a much slower reaction step takes place. If the study is to go beyond the adsorption step, the reaction must be of the type that produces a change in pressure at constant volume and temperature. Figure 4 shows portions of a typical adsorption reaction history for the catalytic dehydration of t-butanol on Alumina lOOS which has been treated or "conditioned" with water (6). The reaction which is endothermic produces one mole of isobutylene and a mole of water for each mole of t-butanoL The steep decrease in pressxore during the first second (approximately) was caused by adsorption, then the slow rise resulted from the reaction. The ratio of adsorption rate to reaction rate for this case was about 1700. The temperature rose during the first three seconds as a result of the heat of adsorption then fell because of the endothermic reaction and heat loss to the reactor. The temperature lag may be due in part to the slower response of the thermocouple. The amount of t-butanol which was measured by the drop in pressure from the initial value to the minimum is considered to be the adsorption at reaction conditions. 

The use of a non-pervaporative extractor-type catalytic polymeric membrane reactor has been reported for light alcohol/acetic acid esterifications. A cross-linked poly(styrene sulfonic acid) (PSA)/PVA blend flat membrane was assembled in the reactor in a vertical configuration, separating two chambers. One of the chambers was loaded with an aqueous solution of ethanol and acetic acid, while the other chamber was filled with chlorobenzene. The esterification equilibrium is displaced to the product s side by the continuous extraction of the formed ester. In the esterifications of methanol, ethanol and n-propanol with acetic acid, the reactivity through the PSA/PVA membrane was higher than that with HCl as catalyst. In that of n-butanol with acetic acid, however, it was viceversa. 

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