Methanol/water separation

Fig. 7. Extractive distillation column profiles for the acetone—methanol—water separation (40). (a) Liquid composition versus theoretical tray location where...

Methanol/water separation, 390 Methylcyclohexane/toluene/plienol separation, 421... 

Figure 17.3. Specifications for a methanol-water separation process.

Concerning the first question, there are many more distillation columns that use singleend temperature control than use dual-temperature control. This is the standard control structure in the methanol/water separation. Using the reflux-to-feed ratio scheme and a single temperature result in energy consumption that is almost the minimum possible by using dual-composition control in the methanol/water system. Instrumentation complexity and loop interaction are avoided. So the structure used in this paper is widely applied in industrial columns. 

Even thou the reaction was conducted for a long time to ccdlect enoi pedymer for characterization, polymer formation was visually observable in only 5 minutes. From viscosity measurements of the red-orange pedymer isolated from the reaction mixture, the avarage molecular wei t was found to be 3(XK). Fractional precipitation by methanol and methanol-water separated the polymer into fractions of molecular weight from 4000 to 2700 which had identical NMR and IR spectra though different melt-softening temperatures (155—167 °C, 110-112 °C, 55-76 C). X-ray diffraction did not show any crystallinity. The results are summarized in Table 4. 

In Chapter 8 we explored the steady-state design of the TAME reactive distiUalion system. The reactive column is part of a multiunit process that includes other columns for recovery of the methanol reactant. The recovery is necessary because the presence of methanol/C5 azeotropes unavoidably removes methanol from the reactive column in the distillate stream. The economics of two alternative methanol recovery systems were evaluated in Chapter 8. In this chapter the dynamic control of the process is studied, and an effective plantwide control structure is developed. The process has three distillation columns one reactive column, one extractive distillation column, and one methanol/water separation column from which methanol and water are recycled. 

In a conventional gasoline containing hydrocarbons or even ethers, the presence of water is not a problem in fact, water is totally soluble up to about 50 ppm at ambient temperature. Beyond this value water separates without affecting the hydrocarbon phase and the water leg can be withdrawn if necessary. On the other hand, in the presence of alcohols (ethanol and especially methanol), trace amounts of water can cause a separation of two phases one is a mixture of water and alcohol, the other of hydrocarbons (Cox, 1979). 

In the United States, the Clean Air Act of 1970 imposed limitations on composition of new fuels, and as such methanol-containing fuels were required to obtain Environmental Protection Agency (EPA) waivers. Upon enactment of the Clean Air Act Amendments of 1977, EPA set for waiver unleaded fuels containing 2 wt % maximum oxygenates excluding methanol (0.3 vol % maximum). Questions regarding methanol s influence on emissions, water separation, and fuel system components were raised (80). 

Reversed-phase hplc has been used to separate PPG into its components using evaporative light scattering and uv detection of their 3,5-dinitroben2oyl derivatives. Acetonitrile—water or methanol—water mixtures effected the separation (175). Polymer glycols in PUR elastomers have been identified (176) by pyrolysis-gc. The pyrolysis was carried out at 600°C and produced a small amount of ethane, CO2, propane, and mostiy propylene, CO, and CH4. The species responsible for a musty odor present in some PUR foam was separated and identified by gc (Supelco SP-2100 capillary column)... 

Silica gel, per se, is not so frequently used in LC as the reversed phases or the bonded phases, because silica separates substances largely by polar interactions with the silanol groups on the silica surface. In contrast, the reversed and bonded phases separate material largely by interactions with the dispersive components of the solute. As the dispersive character of substances, in general, vary more subtly than does their polar character, the reversed and bonded phases are usually preferred. In addition, silica has a significant solubility in many solvents, particularly aqueous solvents and, thus, silica columns can be less stable than those packed with bonded phases. The analytical procedure can be a little more complex and costly with silica gel columns as, in general, a wider variety of more expensive solvents are required. Reversed and bonded phases utilize blended solvents such as hexane/ethanol, methanol/water or acetonitrile/water mixtures as the mobile phase and, consequently, are considerably more economical. Nevertheless, silica gel has certain areas of application for which it is particularly useful and is very effective for separating polarizable substances such as the polynuclear aromatic hydrocarbons and substances... 

Bisethylenedioxypregn-5-ene. Method A. A mixture of progesterone (10 g), freshly distilled ethylene glycol (80 ml) and benzene (350 ml) is slowly distilled for 15 min to remove traces of water. p-Toluenesulfonic acid monohydrate (0.3 g) is added and the mixture is heated under reflux with stirring for 5 hr with a water separator. Saturated sodium bicarbonate solution is added to the cooled mixture and the benzene layer is separated. The organic layer is washed twice with water, dried and evaporated in vacuo. The residue is crystallized twice from acetone-methanol to give 4.15 g (32%) of bisketal, mp 178-181°. 

Acetylene and Potassium in Liquid Ammonia Potassium (40 g) is dissolved in 1 liter of dry liquid ammonia. Dry acetylene is then bubbled into the solution until the blue color is discharged. A solution of 15 g of estrone in 300 ml of dioxane is prepared and diluted with 300 ml of ether, cooled, and added to the potassium acetylide solution over a period of 10 min. The liquid ammonia is allowed to evaporate, an additional 500 ml of ether is added, and the mixture is allowed to stand overnight. About 3 liters of 5 % sulfuric acid is added and the organic layer separated. The water layer is re-extracted with fresh ether, and the combined ether extracts are washed twice with 5 % sodium carbonate solution, th6n several times with water, and finally evaporated under reduced pressure. The residue is dissolved in 150 ml of methanol, then an equal quantity of hot water is added and the mixture cooled. The precipitated solid is collected, washed with cold 60 % methanol and crystallized once from methanol-water to give 14.8 g (85%) of 17a-ethynylestradiol mp 143-144°. 

PVP K-15 and K-30 peaks are symmetric in water and water/methanol, except for the TSK GM-PWxl column in water. This suggests an interaction between PVP K-15 and K-30 with the TSK GM-PWxl column in water. System peaks overlap with the low molecular weight tails of the PVP K-15 and K-30 peaks for all four columns in water. In water/methanol the separation of the system peaks from the polymer peaks is much better for all four columns. 

A mixture of 39.0 grams (0.2 mol) of a-methylhomoveratrylamine and 42.0 grams (0.2 mol) of 3-methoxy-4-ethoxyphenylacetic acid is heated at 190°-200°C for one hour. The reaction mixture is poured into about 100 cc of petroleum ether, whereupon crystals of N-(a-methyl-homoveratryl)-3-methoxy-4-ethoxyphenylacetamide separate. The precipitate is filtered off, and recrystallized from 50% methanol-water. 

Ben2yloxyindolyl-3)-Q -acetvlamino-Q -methylthiopropionic acid methanethiol ester (449 mg) was added to 10 ml of ethanol and further 1 ml of triethylamine was added to the mixture. Then, the reaction mixture was refluxed for 17 hours, after condensation under reduced pressure and subsequent separation of the residue by column chromatography (silica gel, ethyl acetate), 353 mg of methyl -(5-benzyloxyindolyl-3)-Q -acetylamino-Q -methylthio-propionate was obtained as colorless glasslike substance in the yield of 81.5%. Recrystallization of the substance from methanol water afforded 287 mg of crystals. 

However, it was not until the beginning of 1994 that a rapid (<1.5 h) total resolution of two pairs of racemic amino acid derivatives with a CPC device was published [124]. The chiral selector was A-dodecanoyl-L-proline-3,5-dimethylanilide (1) and the system of solvents used was constituted by a mixture of heptane/ethyl acetate/methanol/water (3 1 3 1). Although the amounts of sample resolved were small (2 ml of a 10 inM solution of the amino acid derivatives), this separation demonstrated the feasibility and the potential of the technique for chiral separations. Thus, a number of publications appeared subsequently. Firstly, the same chiral selector was utilized for the resolution of 1 g of ( )-A-(3,5-dinitrobenzoyl)leucine with a modified system of solvents, where the substitution of water by an acidified solution... 

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