Water continued purification

Acid waste waters from silicone production enter neutraliser 9, a concrete container with two agitators, lined with acid-resistant tile from epoxy resin. Here the waste waters are neutralised with lime milk, which is automatically sent from reservoirs 6 with pumps 8. The pumps automatically switch off when pH in the neutraliser is 8-10 and switch on when pH is below 5. Neutral waste waters continuously self-flow through a collector into receiving reservoir 10 as they accumulate, they are automatically sent with pumps 11 for averaging and mechanical purification. 

Titanium tetrachloride can also be purified from impurities by the continuous technique. The installation for continuous purification consists of several vertical pipe coolers. Liquid products of the reaction are sent into the first cooler, which is located a little higher than the rest, where the mixture is cooled at agitation to -3 - -5°C. After that, the mixture is abruptly cooled to -20 - -23.5 °C the solution deposits crystals of Si2Cl6 and VOCI3. The deposited crystals remain in the primary cooler, and the solution self-flows into the secondary coolers, where it is gradually cooled from -23 to -27 °C titanium tetrachloride deposits as white sediment. It is collected in the secondary coolers and washed with water. The TiCl4 thus purified is 99.92% pure. 

Granulated activated carbon is thus preferred, if a high volume stream continuous purification operation makes it necessary. Thus gas purification is almost exclusively carried out in fixed-bed adsorbers with granulated carbon. Potable water in Western Europe and Japan is preferably freed of organic impurities by percolation over granulated activated carbon. 

If the mass should become slrupy instead of crystalline, the evaporation is discontinued and the mixture is diluted in 400-500 ml. of water. Then dilute ammonia is carefully added until the yellow end-point of tropeolin 00, 30 ml. of 2N HCl is added, and the volxame is made up to 600 ml. with water. The purification procedure is then continued as described below.)... 

Filtration is the separation of two phases, particulate form, ie, soHd particles or Hquid droplets, and continuous, ie, Hquid or gas, from a mixture by passing the mixture through a porous medium. This article discusses the more predominant separation of soHds from Hquids. Filtration of soHd particles or Hquid droplets from gases is dealt with elsewhere (see Airpollution controlmethods). The oldest recorded appHcations of filtration are the purifications of wine and water practiced by the ancient Greeks and Romans. Cake filters, such as the rotary vacuum filter and the filter press, were developed much later from the necessity to filter sewage. 

The sweet water from continuous and batch autoclave processes for splitting fats contains tittle or no mineral acids and salts and requires very tittle in the way of purification, as compared to spent lye from kettle soapmaking (9). The sweet water should be processed promptly after splitting to avoid degradation and loss of glycerol by fermentation. Any fatty acids that rise to the top of the sweet water are skimmed. A small amount of alkali is added to precipitate the dissolved fatty acids and neutralize the liquor. The alkaline liquor is then filtered and evaporated to an 88% cmde glycerol. Sweet water from modem noncatalytic, continuous hydrolysis may be evaporated to ca 88% without chemical treatment. 

The gases leaving the purification system are scmbbed with water to recover solvent and a continuous small purge of solvent gets rid of polymers. The acetylene purity resulting from this system is 99%. The main impurities in the acetylene are carbon dioxide, propadiene, and a very small amount of... 

The primary water specifications for a PWR are given in Table 1 (4). Rigid controls are appHed to the primary water makeup to minimise contaminant ingress into the system. In addition, a bypass stream of reactor coolant is processed continuously through a purification system to maintain primary coolant chemistry specifications. This system provides for removal of impurities plus fission and activated products from the primary coolant by a combination of filtration (qv) and ion exchange (qv). The bypass stream also is used both to reduce the primary coolant boron as fuel consumption progresses, and to control the Li concentrations. 

Other Uses. The quantity of coal used for purposes other than combustion or processing is quite small (2,6). Coal, especially anthracite, has estabHshed markets for use as purifying and filtering agents in either the natural form or converted to activated carbon (see Carbon). The latter can be prepared from bituminous coal or coke, and is used in sewage treatment, water purification, respirator absorbers, solvent recovery, and in the food industry. Some of these markets are quite profitable and new uses are continually being sought for this material. 

Process Water Purification Boiler feed water is a major process apphcation of RO. Sealants and colloids are particularly well rejected by membranes, and TDS is reduced to a level that makes ion exchange or continuous deionization for the residual ions very economic. Even the extremely high quahty water required for nuclear power plants can be made from seawater. The iiltra-high quahty water required for production of electronic microcircuits is usually processed starting with two RO systems operating in series, followeci by many other steps. 

The reaction mixture is diluted with 250 ml of water, the mixture is transferred to a 2 liter flask using methanol as a wash liquid, and the organic solvents are distilled at 20-25 mm using a rotary vacuum evaporator. The product separates as a solid and distillation is continued until most of the residual toluene has been removed. The solid is collected on a 90 cm, medium porosity, fritted glass Buchner funnel and washed well with cold water. After the material has been sucked dry, it is covered with a little cold methanol, the mixture is stirred to break up lumps, and the slurry is kept for 5 min. The vacuum is reapplied, the solid is rinsed with a little methanol followed by ether, and the material is air-dried to give 9.1 g (85%), mp 207-213° after sintering at ca. 198°. Reported mp 212-213°. The crude material contains 1.0-1.5% of unreduced starting material as shown by the UV spectrum. Further purification may be effected by crystallization from methanol. 

A solution of sodium methoxide, prepared from sodium (23 g) and dry methanol (500 mL), was added drop-wise at 0 °C to a stirred suspension of aminoacetonitrile hydrochloride (18, 100 g, 1.08 mol) in dry methanol (100 rnL). After stirring for 2 h at rt the precipitated sodium chloride was filtered off and the filtrate concentrated in vacuo. EtOAc (20 mL) was added and evaporated under reduced pressure to remove all traces of methanol. The oily residue was dissolved in dry EtOAc (100 mL) and anhydrous sodium sulfate added. After cooling, the precipitate was filtered off. The solution of crude aminoacetonitrile was used without further purification. This solution was added drop-wise during a period of 1 h to a vigorously stirred, ice-cooled solution of carbon disulphide (100 mL, 1.66 mol) in dry EtOAc (100 mL) under an N2 atmosphere. Continued mechanical stirring and water-free conditions were essential. The mixture was stirred at 0 °C for 1 h. The resultant precipitate was filtered off, washed with EtaO and dried, giving the product 50 as yellow crystals (99 g, 75 % on amount of sodium), m.p. 131 °C dec. IR (KBr) v max 1630, 1500 cm. ... 

A mixture of 1.38 grams of the above compound and 15 cc of dioxane was treated with 1.9 cc of a 0.5 N aqueous solution of perchloric acid and 600 mg of N-bromoacetamide, adding the latter in the dark, in three portions, in the course of half an hour and under continuous stirring. It was then stirred for a further 1% hours in the dark, then the excess of reagent was decomposed by the addition of aqueous sodium bisulfite solution and ice water was added the product was extracted with methylene chloride, washed with water, dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure, thus giving a yellow oil consisting of the 16,21-diacetate of 6a-fluoro-9a-bromo-16o-hydroxy-hydrocortisone which was used for the next step without further purification. 

B. 2-Methylcyclopenlane-l,3,5-trione hydrate. A mixture of 200 g. (0.89 mole) of the keto ester prepared above, 910 ml. of water, and 100 ml. of 85% phosphoric acid is healed under reflux for 4 hours and then cooled in an ice-salt bath to —5°. The trione mixed with oxalic acid separates and is collected by filtration and dried under reduced pressure. The dried material is extracted with boiling ether (250-300 ml.) under reflux, and the ethereal extract is separated from the undissolved oxalic acid. The original aqueous filtrate is also extracted with ether in a continuous extractor. The two extracts are combined, and ether is removed by distillation. The crude trione separates as a dark brown solid and is crystallized from ca. 250 ml. of hot water. The once-crystallized, faintly yellow product weighs 95-105 g. (74-82%), m.p. 70-74°. This product is used in the next step without further purification. A better specimen, m.p. 77-78°, which is almost colorless, can be obtained by recrystallization from hot water after treatment with Norit activated carbon. 

A mixture of 2.0 mmol of a 1.6 N solution of butyllithium in hexane and 0.47 g (2.0 mmol) of(-)-spartcinc in 10 mL of diethyl ether is stirred for 15 min at — 78 rC then 0.26 g (2.0 mmol) of 1-methyl-l//-indene in 2 mL of diethyl ether are added. Stirring is continued for 30 inin at 20 °C, the mixture is cooled to — 70 CC and 2.5 mmol of the acid chloride in 2 mL of diethyl ether are added. After stirring for 4h the usual aqueous workup was accomplished by addition of 10 mL of diethyl ether and successive washing with 10 mL of 2 N aq HC1. water and sat. aq NtiCl, respectively, followed by chromatographic purification on silica gel with diethyl cthcr/pentane. 

Stirring is continued for 2 hours at room temperature, and then methanol is added until a clear solution is obtained (ca. 10 ml. of methanol is required, and some heat is generated). When the solution has cooled, it is washed successively with 200 ml. of aqueous 2N potassium carbonate and 200 ml. of water. The aqueous phases are combined, washed with three 100-ml. portions of chloroform, and discarded. The organic phases are then combined, dried over sodium sulfate, and decolorized with activated carbon. Concentration of the chloroform solution thus obtained provides three crops of pale yellow crystals, which are washed with 30% hexane in chloroform and dried for 2 hours at 80°/0.1 mm. The total yield of 3-(2-phenyl-l,3-dithian-2-yl)indole is 22.3-25.4 g. (72-81%), m.p. 167-169° (Note 7). This material requires no further purification for use in Parts D or E. 

Dimethylphenylsilyl lithium (1 mmol, above THF solution) was added to copper(i) iodide (0.5 mmol) at — 23 °C, and the mixture was stirred at this temperature for 4h. The enone (0.75-0.5mmol) was then added, and stirring was continued at —23 °C for 0.5 h. The mixture was then poured on to ice(25 g)/HCl(5 ml), and extracted with chloroform (3 x 25 ml). The combined extracts were filtered, washed with HCI (25ml, 3m), water (25 ml), saturated sodium hydrogen carbonate solution (25 ml) and water (25 ml), and dried. Concentration and purification by preparative t.l.c. (eluting solvent 3 7 ether petrol) gave the /J-silylketone (40-99%). 

Adipic acid, 219.2 g (1.5 mol), and 77.6 g (1.25 mol) of 1,2-ethanediol are weighed into a 500-mL glass reactor equipped with a mechanical stirrer, a nitrogen inlet, and a distillation head connected to a condenser and a receiver fiask. The reactor is placed in a salt bath preheated at 180°C and the temperature is dien raised gradually to 220°C (see note at end of procedure) until the greater part of water has been removed (3 h). The reactor is cooled down to 160°C and vacuum is applied slowly to ca. 0.07 mbar (30 min). Temperature is ramped to 220°C (see note below) at a rate of l°C/min and reaction is continued for an additional 90 min. At the end of reaction, the carboxylic acid endgroup content is close to 1.90 mol/kg. No purification of final polyester is carried out. 

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