Liquid products appearance

Figure 12 clearly shows the effect of iron sulfide content of the coal on total conversion and liquid product yield during hydrogenation. The conversion increased from about 52 per cent to 70 per cent using the hot-rod reactor with no added catalyst. The yield of toluene soluble product (oil plus asphaltene) increased from about 30 to 44 per cent with total sulfur increase from 1 to 6.5 per cent. Thus it would appear that iron sulfide can act catalytically in the dry hydrogenation reaction as well as in slurried reactions (15). 

After reaction, any solid residue was filtered off and the liquid product was separated by distillation into a bottoms product and a distillate that included unreacted Tetralin and low-boiling products from both the coal and the Tetralin. As tetralin breaks down under dissolution conditions to form mainly the tetralin isomer 1-methyl indan, naphthalene and alkyl benzenes (4) it was assumed that no compound with a higher boiling point than naphthalene was formed from the solvent, and the distillation to recover solvent was therefore continued until naphthalene stopped subliming. Some residual naphthalene remained in the bottoms product its mass, as determined from nmr and elemental analysis, was subtracted from the mass of bottoms product recovered and included in the amount of distillate recovered. It was assumed that all naphthalene present came from the Tetralin, not the coal. However, as the amount of tetralin reacted was 10 times the amount of coal this assumption appears reasonable. 

The reactions of Eq. (2) could not be carried to completion in a reactive olefin such as 1-hexene. After several increments of MeCl2SiH had been added to the mixture, succeeding increments were mostly consumed to form /i-C6H13MeSiCl2. When this product appeared in the solution, gas-liquid chromatography (GLC) showed that hexene in the solution was no longer only 1-hexene but a mixture of isomers which contained mostly 2- and-3-hexene, in both cis and trans conformations. 

The principal competing reactions to ruthenium-catalyzed acetic acid homologation appear to be water-gas shift to C02, hydrocarbon formation (primarily ethane and propane in this case) plus smaller amounts of esterification and the formation of ethyl acetate (see Experimental Section). Unreacted methyl iodide is rarely detected in these crude liquid products. The propionic acid plus higher acid product fractions may be isolated from the used ruthenium catalyst and unreacted acetic acid by distillation in vacuo. 

We remember that neither solids, such as Ca5(P04)30H(s), nor liquids, such as H20(1), appear in the equilibrium constant expression. Concentrations of products appear in the... 

Your solid products should not be gray. Liquid products (yes, you can do liquids ) will let you know that you didn t get all the charcoal out. Often, you can t see charcoal contamination in liquids while you re working with them. The particles stay suspended for awhile, but after a few days, you can see a layer of charcoal on the bottom of the container. Sneaky, those liquids. By the time the instructor gets to grade all the products—voila—the charcoal has appeared. 

Radiolysis of CO, both in the liquid and gaseous states, also leads to C02 and C302 formation, the latter product appearing mainly as a polymeric solid23-27. A scheme of reactions consisting of the initial production of a carbon and an oxygen atom, followed by (10)-(12) and... 

The reaction of Li2PH in DME leads preferentially to compounds 9 and 10, which appear as a white powder, from which compound 9 can be obtained as cubic crystals by recrystallization with pentane or toluene. The presence of Me2Si(PH2)Cl (1), Me2Si(PH2)2 (2), as well as 3,4,5,6, 7, and 8 can be demonstrated in the liquid products of the reaction (34). 

B. 4-Phenyl-l-carbethoxysemicarbazide. In a 1-1. three-necked round-bottomed flask equipped with a liquid-sealed mechanical stirrer (Note 3), a constant-pressure dropping funnel, and a reflux condenser fitted with a drying tube containing silica gel is placed a solution of 52 g. (0.5 mole) of ethyl hydrazine-carboxylate in 550 ml. of dry benzene (Note 4). The solution is cooled in an ice bath, and the stirrer is started. To the solution is added 59.7 g. (55 ml., 0.5 mole) of phenyl isocyanate (Note 5) dropwise over a period of 45 minutes. After about one-half of the isocyanate has been added, a white precipitate of the product appears, and the reaction mixture becomes progressively thicker. After addition is complete the ice bath is removed, and the mixture is stirred at room temperature for 2 hours and then is heated under reflux for 2 hours. The suspension is allowed to cool to room temperature, and 4-phenyl-1-carbethoxysemi-carbazide is isolated by suction filtration, washed with 500 ml. of benzene, and dried in a vacuum desiccator. The yield is 108 g. (97%), m.p. 151-152°. The product is not further purified before being used in the next step. It may be recrystallized from ethyl acetate to yield white crystals, m.p. 154-155°, vmax 1645, 1687, 1797, and 3300 cm.-1 (Note 6). 

The liquid and solid products of the reaction were collected and measured after the head of the cylinder had been removed, the liquid products being drawn off into a measuring vessel and the solid products scraped out and weighed. Since secondary reactions might take place as soon as the air struck the products, the material collected might not be identical with that immediately resulting from the reaction however, no better method appears to have been devised... 

Examples from the patent literature, as shown in Expts. B and C of Table VI, are generally found to contain possible secondary products in much lower proportions. These examples illustrate selectivities to the two major primary products, methanol and ethylene glycol, of greater than 90%. The higher proportion of probable secondary products in Expt. A would appear to be a result of carrying out this reaction to very high product concentrations the volume of liquid products formed during the experiment is approximately equal to the initial volume of solvent. Results of experi-... 

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