Water, continuous removal

Glucose 1 mol + fatty alcohol 3-10 mol —> mono alkyl glucoside + water (continually removed)... 

Perhaps the simplest case of reaction of a solid surface is that where the reaction product is continuously removed, as in the dissolving of a soluble salt in water or that of a metal or metal oxide in an acidic solution. This situation is discussed in Section XVII-2 in connection with surface area determination. 

Continue the passage of bromine vapour until the solution in A assumes a distinctly yellow colour (2-3 hours) the reaction is then complete. Filter the tribromoaniline on a Buchner funnel, wash it thoroughly with water to remove hydrobromic acid, and suck as dry as possible. Ilecr3 stallise from methylated (or rectified) spirit. The yield is 22 g. m.p. 120°. 

Chlorodiphenyl. Diazotise 32 g. of o-chloroaniline (Section IV,34) in the presence of 40 ml. of concentrated hydrochloric acid and 22 -5 ml. of water in the usual manner (compare Section IV,61) with concentrated sodium nitrite solution. Transfer the cold, filtered diazonium solution to a 1 5 htre bolt-head flask surrounded by ice water, introduce 500 ml. of cold benzene, stir vigorously, and add a solution of 80 g. of sodium acetate trihydrate in 200 ml. of water dropwise, maintaining the temperature at 5-10°. Continue the stirring for 48 hours after the first 3 hours, allow the reaction to proceed at room temperature. Separate the benzene layer, wash it with water, and remove the benzene by distillation at atmospheric pressure distil the residue under reduced pressure and collect the 2-chlorodiphenyl at 150-155°/10 mm. The yield is 18 g. Recrystalliae from aqueous ethanol m.p. 34°. 

Small amounts of propionitrile and bis(cyanoethyl) ether are formed as by-products. The hydrogen ions are formed from water at the anode and pass to the cathode through a membrane. The catholyte that is continuously recirculated in the cell consists of a mixture of acrylonitrile, water, and a tetraalkylammonium salt the anolyte is recirculated aqueous sulfuric acid. A quantity of catholyte is continuously removed for recovery of adiponitrile and unreacted acrylonitrile the latter is fed back to the catholyte with fresh acrylonitrile. Oxygen that is produced at the anodes is vented and water is added to the circulating anolyte to replace the water that is lost through electrolysis. The operating temperature of the cell is ca 50—60°C. Current densities are 0.25-1.5 A/cm (see Electrochemical processing). 

Water is continuously added to the last extraction bath and flows countercurrenfly to filament travel from bath to bath. Maximum solvent concentration of 15—30% is reached in the coagulation bath and maintained constant by continuously removing the solvent—water mixture for solvent recovery. Spinning solvent is generally recovered by a two-stage process in which the excess water is initially removed by distillation followed by transfer of cmde solvent to a second column where it is distilled and transferred for reuse in polymer manufacture. 

Another process employs a pH maintained at 4—7 and a catalyst that combines a divalent metal cation and an acid. Water is removed continuously by azeotropic distillation and xylene is recycled. The low water content increases the reaction rate. The dibenzyl ether groups are decomposed by the acid the yield of 2,2 -methylene can be as high as 97% (34). 

During calcination, water is removed at temperatures between 200 and 300°C sulfur trioxide is removed at temperatures between 480 and 800°C. At about 480°C the crystals of Ti02 are being formed and continue to grow with increasing temperature. To prepare the anatase pigment, the final calcination temperature of the hydrolysate prepared in the presence of anatase seeds should reach about 800—850°C. 

Nylon-11. This nylon is produced from 11-aminoundecanoic acid, which is derived from castor oil. The acid is polymerized by heating to 200°C with continuous removal of water. Catalysts such as phosphoric acid are frequentiy used. There is no appreciable amount of unreacted monomer left in the product. 

Solvent Process. In the solvent process, or solvent cook, water formed from the reaction is removed from the reactor as an a2eotropic mixture with an added solvent, typically xylene. Usually between 3 to 10 wt % of the solvent, based on the total charge, is added at the beginning of the esterification step. The mixed vapor passes through a condenser. The condensed water and solvent have low solubiUty in each other and phase separation is allowed to occur in an automatic decanter. The water is removed, usually to a measuring vessel. The amount of water collected can be monitored as one of the indicators of the extent of the reaction. The solvent is continuously returned to the reactor to be recycled. Typical equipment for this process is shown in Figure 2. The reactor temperature is modulated by the amount and type of refluxing solvent. Typical conditions are ... 

Commercial and Artificial Processing. Commercially, silkworm cocoons are extracted in hot soapy water to remove the sticky sericin protein. The remaining fibroin or stmctural sdk is reeled onto spools, yielding approximately 300—1200 m of usable thread per cocoon. These threads can be dyed or modified for textile appUcations. Production levels of sdk textiles in 1992 were 67,000 metric tons worldwide. The highest levels were in China, at 30,000 t, foUowed byJapan, at 17,000 t, and other Asian and Oceanian countries, at 14,000 t (24). Less than 3000 metric tons are produced annually in each of eastern Europe, western Europe, and Latin America almost no production exists in North America, the Middle East, or Africa. 1993 projections were for a continued worldwide increase in sdk textile production to 75,000 metric tons by 1997 and 90,000 metric tons by 2002 (24). 

Processes to produce boric acid esters are based on the azeotropic removal of water from a mixture of the appropriate alcohol, phenol, or glycol, and boric acid. A suitable hydrocarbon azeotroping agent is used to help remove the water. The water is removed continuously by using a condenser that allows continuous return of the solvent to the reaction vessel. Eor some borate esters, such as the glycol borates, distillation can result in decomposition. 

Catalysts used are usually acids such as sulfuric acid, -toluenesulfonic acid, sulfonic acid ion-exchange resins, and others. The water from the reaction of the citric acid and the alcohol is continuously removed as the azeotrope until no more water is formed. At this point, the reaction is usually complete and the solvent and any excess alcohol is distilled off under mild vacuum. The catalyst is neutralized using carbonate or sodium hydroxide, leaving a cmde product. If a pure product is desired, the ester can be distilled under high vacuum. 

A continuous distillation process has been studied for the production of high boiling esters from intermediate boiling polyhydric alcohols and low boiling monocarboxyhc aUphatic or aromatic acids (56). The water of reaction and some of the organic acid were continuously removed from the base of the column. 

To rinse, wash the surface in clear, continuous running water to remove all traces of degreasing agent from the surface. Two/three dips at room temperature are sufficient. 

Valeric acid (n-pentanoic acid) [109-52-4] M 102.1, b 95 /22mm, 186.4 /atm, d 0.938, n 1.4080, pK 4.81. Water was removed from the acid by distn using a Vigreux column, until the boiling point reached 183 . A few crystals of KMn04 were added, and after refluxing, the distn was continued, [Andrews and Keefer 7 Am Chem Soc 83 3708 1961.]... 

When the addition is completed, the bath is removed and stirring is continued for 1 hour while the reaction mixture gradually cools to room temperature. Sodium carbonate (100 g.) is added in portions, followed by the cautious addition of 60 g. of sodium bicarbonate (Note 3). The water is removed from the slightly basic solution by heating the solution in a 3-1. round-bottomed flask under reduced pressure on a steam bath. To aid in removing the last traces of water, 250 ml. of ethanol is added to the residue and the mixture is heated under reduced pressure on a steam bath until it ajipcars dry (Note 4). 

Most glycol dehydration processes are continuous. That is, gas and glycol flow continuously through a vessel (the contactor" or absorber ) where they come in contact and the glycol absorbs the water. The glycol flows from the contactor to a reboiler (sometimes called "reconcentrator or regenerator where the water is removed or stripped from the glycol and is then pumped back to the contactor to complete the cycle. 

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