Wash water

Add 23 g. of powdered (or flake ) sodium hydroxide to a solution of 15 ml. (18 g.) of nitrobenzene in 120 ml. of methanol contained in a 250 ml. short-necked bolt-head flask. Fix a reflux water-condenser to the flask and boil the solution on a water-bath for 3 hours, shaking the product vigorously at intervals to ensure thorough mixing. Then fit a bent delivery-tube to the flask, and reverse the condenser for distillation, as in Fig. 59, p. 100, or Fig. 23(D), p. 45). Place the flask in the boiling water-bath (since methanol will not readily distil when heated on a water-bath) and distil off as much methanol as possible. Then pour the residual product with stirring into about 250 ml. of cold water wash out the flask with water, and then acidify the mixture with hydrochloric acid. The crude azoxybenzene separates as a heavy oil, which when thoroughly stirred soon solidifies, particularly if the mixture is cooled in ice-water. 

When the reaction is complete, heat the stirred mixture carefully under reflux over a Bunsen burner and asbestos gauze for I hour if the mixture becomes too thick for efficient stirring, add up to 15 mL of acetic acid. Now decant the hot mixture into 500 ml. of vigorously-stirred ice-cold water wash the residual zinc thoroughly with glacial acetic acid (2 portions each of I -2 ml.), decanting the acid also into the stirred water. 

Ethyl n-butyrate. Use a mixture of 88 g. (92 ml.) of n-butyric acid, 23 g. (29 ml.) of ethanol and 9 g. (5 ml.) of concentrated sulphuric acid. Reflux for 14 hours. Pour into excess of water, wash several times with water, followed by saturated sodium bicarbonate solution until all the acid is removed, and finally with water. Dry with anhydrous magnesium sulphate, and distU. The ethyl n-but3rrate passes over at 119 5-120-5°, Yield 40 g. An improved yield can be obtained by distilhng the reaction mixture through an efficient fractionating column until the temperature rises to 125°, and purifying the crude ester as detailed above under methyl acetate. 

Dissolve 1 0 g. (or 10 ml.) of the amine and 1 0 g. of 2 4-dinitrochloro-benzene in 5-10 ml. of ethanol, add a slight excess of anhydrous potassium carbonate or of powdered fused sodium acetate, reflux the mixture on a water bath for 20-30 minutes, and then pour into water. Wash the precipitated solid with dilute sodium carbonate solution, followed by dilute hydrochloric acid. Recrystallise from ethanol, dilute alcohol or glacial acetic acid. 

Added 112 grams sassafras oil. Shake for a couple of minutes. You get an orangish emulsion. Clears within 15 minutes forming two layers, bottom layer oil, top layer acetic acid, eugenol + the other solubles. Separated the oil from the others, washed the oil layer 2x with fresh C//-/2O. Weight after acetic acid water washes 101.5 (-10.5 grams). 

To separate the oil added an equal volume of fresh cool water (note waited until solution cooled before adding the water). The oil started to drop out perfectly, used DCM to extract all traces of the oil. This woik up is by far the cleanest, easiest and simplest to date... (This dreamer was tried all method of ketone synthesis)... Once the oil was extracted, the extracts were pooled washed with sodium bicarbonate lx, saturated solution of NaCI 1x, and two washes with fresh dHzO... Some time was required for the work up as there was a little emulsion from the use of the base wash and then with the first water wash. The JOC ref suggested using an alumina column to remove the catalyst (could be a better way to go). 

The equation above suggests that one approach would be to use a pore Hquid that has a low surface tension. Indeed, two-step acid—base or acid—acid catalyzed sHica gels have been made, aged in ethanol or water, washed with various aprotic solvents, and finally evaporatively dried at 323 K for 48 hours and then at 383 K for 48 hours (43). The aprotic solvents used and their corresponding surface tension in N/m at room temperature (shown in... 

The Biazzi continuous process is also used. The reactants are continuously fed to a series of nitrators at 15—20°C followed by separation of the PETN, water washing, solution in acetone at 50°C, neutralization with gaseous ammonia, and precipitation by dilution with water. The overall yield is more than 95%. The acetone and the spent acid are readily recovered. 

Volatile products may be removed by direct distillation or the soHd magnesium hahde may be removed by filtration, before solvent evaporation. If the final product is not water sensitive, water-washing of the final reaction product mixture usually removes the salts convenientiy. 

Up to 0.4 g/L of the iodine stays in solution and the rest precipitates as crystallized iodine, which is removed by flotation (qv). This operation does not require a flotation agent, owing to the hydrophobic character of the crystallized element. From the flotation cell a heavy pulp, which is water-washed and submitted to a second flotation step, is obtained. The washed pulp is introduced into a heat exchanger where it is heated under pressure up to 120°C to melt the iodine that flows into a first reactor for decantation. From there the melt flows into a second reactor for sulfuric acid drying. The refined iodine is either flaked or prilled, and packed in 50- and 25-kg plastic-lined fiber dmms. 

Naphthalenol. 2-Naphthol or p-naphthol or 2-hydroxynaphthalene/7i3 -/5 -i7 melts at 122°C and boils at 295°C, and forms colorless crystals of characteristic, phenoHc odor which darken on exposure to air or light. 2-Naphthol [135-19-3] is manufactured by fusion of sodium 2-naphthalenesulfonate with sodium hydroxide at ca 325°C, acidification of the drowned fusion mass which is quenched ia water, isolation and water-washing of the 2-naphthalenol, and vacuum distillation and flaking of the product. A continuous process of this type has been patented (69). The high sulfate content ia the primary effluent from 2-naphthol production is greatiy reduced ia modem production plants by the recovery of sodium sulfate. 

Niobic Acid. Niobic acid, Nb20 XH2O, includes all hydrated forms of niobium pentoxide, where the degree of hydration depends on the method of preparation, age, etc. It is a white insoluble precipitate formed by acid hydrolysis of niobates that are prepared by alkaH pyrosulfate, carbonate, or hydroxide fusion base hydrolysis of niobium fluoride solutions or aqueous hydrolysis of chlorides or bromides. When it is formed in the presence of tannin, a volurninous red complex forms. Freshly precipitated niobic acid usually is coUoidal and is peptized by water washing, thus it is difficult to free from traces of electrolyte. Its properties vary with age and reactivity is noticeably diminished on standing for even a few days. It is soluble in concentrated hydrochloric and sulfuric acids but is reprecipitated on dilution and boiling and can be complexed when it is freshly made with oxaHc or tartaric acid. It is soluble in hydrofluoric acid of any concentration. 

The solvent is 28 CC-olefins recycled from the fractionation section. Effluent from the reactors includes product a-olefins, unreacted ethylene, aluminum alkyls of the same carbon number distribution as the product olefins, and polymer. The effluent is flashed to remove ethylene, filtered to remove polyethylene, and treated to reduce the aluminum alkyls in the stream. In the original plant operation, these aluminum alkyls were not removed, resulting in the formation of paraffins (- 1.4%) when the reactor effluent was treated with caustic to kill the catalyst. In the new plant, however, it is likely that these aluminum alkyls are transalkylated with ethylene by adding a catalyst such as 60 ppm of a nickel compound, eg, nickel octanoate (6). The new plant contains a caustic wash section and the product olefins still contain some paraffins ( 0.5%). After treatment with caustic, cmde olefins are sent to a water wash to remove sodium and aluminum salts. 

Idemitsu Process. Idemitsu built a 50 t x 10 per year plant at Chiba, Japan, which was commissioned in Febmary of 1989. In the Idemitsu process, ethylene is oligomerised at 120°C and 3.3 MPa (33 atm) for about one hour in the presence of a large amount of cyclohexane and a three-component catalyst. The cyclohexane comprises about 120% of the product olefin. The catalyst includes sirconium tetrachloride, an aluminum alkyl such as a mixture of ethylalurninumsesquichloride and triethyl aluminum, and a Lewis base such as thiophene or an alcohol such as methanol (qv). This catalyst combination appears to produce more polymer (- 2%) than catalysts used in other a-olefin processes. The catalyst content of the cmde product is about 0.1 wt %. The catalyst is killed by using weak ammonium hydroxide followed by a water wash. Ethylene and cyclohexane are recycled. Idemitsu s basic a-olefin process patent (9) indicates that linear a-olefin levels are as high as 96% at C g and close to 100% at and Cg. This is somewhat higher than those produced by other processes. 

Desalting is a water-washing operation performed at the production field and at the refinery site for additional cmde oil cleanup. If the petroleum from the separators contains water and dirt, water washing can remove much of the water-soluble minerals and entrained soflds. If these cmde oil contaminants are not removed, they can cause operating problems duting refinery processiag, such as equipment plugging and corrosion as well as catalyst deactivation. 

Some producers beneficiate the phosphate ore prior to agglomeration to increase the phosphate content and remove undesirable contaminants. One approach uses a water wash to remove fines which are lower in assay and higher in contamination. If too much clay is removed from the ore by the beneficiation, a binder such as bentonite clay must be added back to the ore to faciUtate agglomeration. 

Propane and light ends are rejected by touting a portion of the compressor discharge to the depropanizer column. The reactor effluent is treated prior to debutanization to remove residual esters by means of acid and alkaline water washes. The deisobutanizer is designed to provide a high purity isobutane stream for recycle to the reactor, a sidecut normal butane stream, and a low vapor pressure alkylate product. 

After epoxidation, propylene oxide, excess propylene, and propane are distilled overhead. Propane is purged from the process propylene is recycled to the epoxidation reactor. The bottoms Hquid is treated with a base, such as sodium hydroxide, to neutralize the acids. Acids in this stream cause dehydration of the 1-phenylethanol to styrene. The styrene readily polymerizes under these conditions (177—179). Neutralization, along with water washing, allows phase separation such that the salts and molybdenum catalyst remain in the aqueous phase (179). Dissolved organics in the aqueous phase ate further recovered by treatment with sulfuric acid and phase separation. The organic phase is then distilled to recover 1-phenylethanol overhead. The heavy bottoms are burned for fuel (180,181). 

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