Acetone purification

Phenol and acetone purification (3) Phenol and acetone are separated and purified. A small amount of byproduct is rejected as heavy residue. 

Figure 4. Acetone by direct oxidation of propene (a) reactor (oxygen), (b) separator, (c) reactor (propene), (d) flash column, (e) light ends distillation, (f) acetone purification.

Absolute methyl alcohol. The synthetic methanol now available is suitable for most purposes without purification indeed, some manufacturers claim a purity of 99 85 per cent, with not more than 0 1 per cent, by weight of water and not more than 0 02 per cent, by weight of acetone. Frequently, however, the acetone content may be as high as 0 1 per cent, and the water content 0-5-1 per cent. 

The solvent used to form the dope is evaporated during the extrusion process and must be recovered. This is usually done by adsorption on activated carbon or condensation by refrigeration. For final purification, the solvent is distilled. Approximately 3 kg of acetone, over 99%, is recovered per kg of acetate yam produced. Recovery of solvent from triacetate extmsion is similar, but ca 4 kg of methylene chloride solvent is needed per kg of triacetate yam extmded. 

Commercial VPO of propane—butane mixtures was in operation at Celanese Chemical Co. plants in Texas and/or Canada from the 1940s to the 1970s. The principal primary products were acetaldehyde, formaldehyde, methanol, and acetone. The process was mn at low hydrocarbon conversion (3—10%) and a pressure in excess of 790 kPa (7.8 atm). These operations were discontinued because of various economic factors, mainly the energy-intensive purification system required to separate the complex product streams. 

Most by-product acetylene from ethylene production is hydrogenated to ethylene in the course of separation and purification of ethylene. In this process, however, acetylene can be recovered economically by solvent absorption instead of hydrogenation. Commercial recovery processes based on acetone, dimetbylform amide, or /V-metby1pyrro1idinone have a long history of successfiil operation. The difficulty in using this relatively low cost acetylene is that each 450, 000 t/yr world-scale ethylene plant only produces from 7000 9000 t/yr of acetylene. This is a small volume for an economically scaled derivatives unit. 

Purification Processes. Separation of neutral and polar Hpids, so-called deoiling, is the most important fractionation process in lecithin technology (Fig. 3). Lecithin is fluidized by adding 15—30% acetone under intensive agitation with acetone (fluidized lecithin acetone, 1 5) at 5°C. The mixture goes to a separator where it is agitated for 30 minutes. The agitator is then stopped and the lecithin separates. The oil micella is removed and the acetone evaporated. After condensation the acetone is returned into the process. 

Recovery and Purification. The dalbaheptides are present in both the fermentation broth and the mycelial mass, from which they can be extracted with acetone or methanol, or by raising the pH of the harvested material, eg, to a pH of 10.5—11 for A47934 (16) (44) and A41030 (41) and actaplanin (Table 2) (28). A detailed review on the isolation of dalbaheptides has been written (14). Recovery from aqueous solution is made by ion pair (avoparcin) or butanol (teicoplanin) extraction. The described isolation schemes use ion-exchange matrices such as Dowex and Amberlite IR, acidic alumina, cross-linked polymeric adsorbents such as Diaion HP and Amberlite XAD, cation-exchange dextran gel (Sephadex), and polyamides in various sequences. Reverse-phase hplc, ion-exchange, or affinity resins may be used for further purification (14,89). 

After flashing the propylene, the aqueous solution from the separator is sent to the purification section where the catalyst is separated by a2eotropic distillation 88 wt % isopropyl alcohol is obtained overhead. The bottoms containing aqueous catalyst solution are recycled to the reactor, and the light ends are stripped of low boiling impurities, eg, diisopropyl ether and acetone. A2eotropic distillation yields dry isopropyl alcohol, and the final distillation column yields a product of more than 99.99% purity. 

Fiaal purification of propylene oxide is accompHshed by a series of conventional and extractive distillations. Impurities ia the cmde product iaclude water, methyl formate, acetone, methanol, formaldehyde, acetaldehyde, propionaldehyde, and some heavier hydrocarbons. Conventional distillation ia one or two columns separates some of the lower boiling components overhead, while taking some of the higher boilers out the bottom of the column. The reduced level of impurities are then extractively distilled ia one or more columns to provide a purified propylene oxide product. The solvent used for extractive distillation is distilled ia a conventional column to remove the impurities and then recycled (155,156). A variety of extractive solvents have been demonstrated to be effective ia purifyiag propylene oxide, as shown ia Table 4. 

Polyethers are usually found in both the filtrate and the mycelial fraction, but in high yielding fermentations they are mosdy in the mycelium because of their low water-solubiUty (162). The high lipophilicity of both the free acid and the salt forms of the polyether antibiotics lends these compounds to efficient organic solvent extraction and chromatography (qv) on adsorbents such as siUca gel and alumina. Many of the production procedures utilize the separation of the mycelium followed by extraction using solvents such as methanol or acetone. A number of the polyethers can be readily crystallized, either as the free acid or as the sodium or potassium salt, after only minimal purification. 

Purification. Enzyme purity, expressed in terms of the percent active enzyme protein of total protein, is primarily achieved by the strain selection and fermentation method. In some cases, however, removal of nonactive protein by purification is necessary. The key purification method is selective precipitation of the product or impurities by addition of salt, eg, sodium sulfate, or solvent, eg, ethanol or acetone by heat denaturation or by isoelectric precipitation, ie, pH adjustments. Methods have been introduced to produce crystalline enzyme preparations (24). 

One of the most important appHcations of this process is that of methyl methacrylate manufacture. In this process (81), acetone cyanohydrin is treated with sulfuric acid at 100°C, affording the corresponding methacrylamide sulfate which is esterified with methanol. After purification, methyl methacrylate (99.8% purity) is obtained in a yield of ca 85%. 

For materials with very low melting points it is sometimes convenient to use dilute solutions in acetone, methanol, pentane, diethyl ether or CHCI3-CCI4. The solutions are cooled to -78° in a dry-ice/acetone bath, to give a slurry which is filtered off through a precooled Buchner funnel. Experimental details, as applied to the purification of nitromethane, are given by Parrett and Sun [J Chem Educ 54 448 7977]. 

Cellulose for chromatography is purified by sequential washing with chloroform, ethanol, water, ethanol, chloroform and acetone. More extensive purification uses aqueous ammonia, water, hydrochloric acid, water, acetone and diethyl ether, followed by drying in a vacuum. Trace metals can be removed from filter paper by washing for several hours with O.IM oxalic or citric acid, followed by repeated washing with distilled water. 

Adipic acid [124-04-9] M 146.1, m 154 , pK 4.44, pK 5.45. For use as a volumetric standard, adipic acid was crystd once from hot water with the addition of a little animal charcoal, dried at 120 for 2h, then recrystd from acetone and again dried at 120 for 2h. Other purification procedures include crystn from ethyl acetate and from acetone/petroleum ether, fusion followed by filtration and crystn from the melt, and preliminary distn under vac. 

The general purification methods listed for xylene are applicable. p-Xylene can readily be separated from its isomers by crystn from such solvents as MeOH, EtOH, isopropanol, acetone, butanone, toluene, pentane or pentene. It can be further purified by fractional crystn by partial freezing, and stored over sodium wire or molecular sieves Linde type 4A. [Stokes and French J Chem Soc, Faraday Trans 1 76 537 1980.]... 

Ruthenium (IV) oxide [12036-10-1] M 133.1, d 6.97. Freed from nitrates by boiling in distilled water and filtering. A more complete purification is based on fusion in a KOH-KNO3 mix to form the soluble ruthenate and perruthenate salts. The melt is dissolved in water, and filtered, then acetone is added to reduce the ruthenates to the insoluble hydrate oxide which, after making a slurry with paper pulp, is filtered and ignited in air to form the anhydrous oxide [Campbell, Ortner and Anderson Anal Chem 33 58 1961]. 

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