Production product acid water

Fig. 23.4. Fig. 23.1 acid plant water requirement as a function of mass% H2S04 in acid plant product acid. Water requirement increases with decreasing specified mass% H2S04 (i.e. with increasing specified mass% FfOt in acid. 

In a widely used industnal process the mixture of ethylene and propene that is obtained by dehydrogenation of natural gas is passed into concentrated sulfunc acid Water is added and the solution IS heated to hydrolyze the alkyl hydrogen sulfate The product is almost exclusively a sin gle alcohol Is this alcohol ethanol 1 propanol or 2 propanoH Why is this particular one formed almost exclusively" ... 

From the intermediate 4, loss of water simply drives the reaction back to starting material, but the water molecule that is eliminated may be H2 0 or H2 0. Therefore, there is a build-up of in the starting material and in the product acid 5. This sort of exchange process was found to be common In many similar systems. 

The reaction solution is flushed under reduced pressure after it is sent out from the column, to remove CO2 gas formed as a by-product. The water formed is then removed from the reaction solution by a2eotropic distillation with BN, and most of the resultant reaction solution is recycled to the reaction column as the circulating solution. Part of the circulating solution is taken out from the reaction system and processed further to obtain DBO. The catalyst is first filtered, then BN, C H OH, and by-products are removed from the resultant solution. Purified DBO is thus obtained. The catalyst, BN, and C4H2OH are recovered and recycled to the circulating solution. After the make-up C H OH and nitric acid are added, the circulating solution is pressuri2ed and fed back to the reaction column. 

Thermal Process. In the manufacture of phosphoric acid from elemental phosphoms, white (yellow) phosphoms is burned in excess air, the resulting phosphoms pentoxide is hydrated, heats of combustion and hydration are removed, and the phosphoric acid mist collected. Within limits, the concentration of the product acid is controlled by the quantity of water added and the cooling capabiUties. Various process schemes deal with the problems of high combustion-zone temperatures, the reactivity of hot phosphoms pentoxide, the corrosive nature of hot phosphoric acid, and the difficulty of collecting fine phosphoric acid mist. The principal process types (Fig. 3) include the wetted-waH, water-cooled, or air-cooled combustion chamber, depending on the method used to protect the combustion chamber wall. 

Hot combustion gases are quenched and saturated with water in a spray chamber called a hydrator. An absorber bed of carbon or graphite rings may be mounted above the hydrator in the same stmcture to obtain more complete absorption of P40 q and to assure that the gas stream is cooled to about 100°C. Weak acid from mist collection is sprayed on the absorber bed, and product acid at 75—85% H PO leaves the hydrator through a heat exchanger. 

Functional derivatives of polyethylene, particularly poly(vinyl alcohol) and poly(acryLic acid) and derivatives, have received attention because of their water-solubility and disposal iato the aqueous environment. Poly(vinyl alcohol) is used ia a wide variety of appHcations, including textiles, paper, plastic films, etc, and poly(acryLic acid) is widely used ia detergents as a builder, a super-absorbent for diapers and feminine hygiene products, for water treatment, ia thickeners, as pigment dispersant, etc (see Vinyl polymers, vinyl alcohol polymers). 

Benzene. The reaction of sulfur trioxide and ben2ene in an inert solvent is very fast at low temperatures. Yields of 90% ben2enesulfonic acid can be expected. Increased yields of about 95% can be reali2ed when the solvent is sulfur dioxide. In contrast, the use of concentrated sulfuric acid causes the sulfonation reaction to reach reflux equiUbrium after almost 30 hours at only an 80% yield. The by-product is water, which dilutes the sulfuric acid estabhshing an equiUbrium. 

There are 10 producers of calcium chloride solutions in the United States, three of these also make a dry product. Solution production is centered around Michigan (brines), California and Utah (brines), and Louisiana (by-product acid). The majority of dry calcium chloride is made in Michigan, lesser quantities in Louisiana, and minor quantities in California. Production involves removal of other chlorides (primarily magnesium) by precipitation and filtration followed by concentration of the calcium chloride solution, either for ultimate sale, or for feed for dry product. Commercial dry products vary by the amount of water removed and by the nature of the drying equipment used. Production and capacity figures for the United States are indicated in Table 2. 

There is no specific color or other reaction by which methyl chloride can be detected or identified. QuaUty testing of methyl chloride for appearance, water content, acidity, nonvolatile residue, residual odor, methanol, and acetone is routinely done by production laboratories. Water content is determined with Kad Fischer reagent using the apparatus by Kieselbach (55). Acidity is determined by titration with alcohoHc sodium hydroxide solution. The nonvolatile residue, consisting of oil or waxy material, is determined by evaporating a sample of the methyl chloride at room temperature. The residue is examined after evaporation for the presence of odor. Methanol and acetone content are determined by gas chromatography. 

The mixed oxidation products are fed to a stiU where the pelargonic and other low boiling acids are removed as overhead while the heavy material, esters and dimer acids, are removed as residue. The side-stream contains predominately azelaic acid along with minor amounts of other dibasic acids and palmitic and stearic acids. The side-stream is then washed with hot water that dissolves the azelaic acid, and separation can then be made from the water-insoluble acids, palmitic and stearic acids. Water is removed from the aqueous solution by evaporators or through crystallization (44,45). 

Dissolve in H2O and acidify with 3N HCl to pH 3.5. Collect the solid and wash with H2O. The air-dried ppte is extracted with 70% aqueous EtOH, filtered hot and cooled slowly. Fine yellow needles of the acid crystallise out, are filtered and dissolved in the minimum quantity of O.OIN NaOH and reppted with N HCl to pH 3.5. It is then recrystd from 70% aqueous EtOH (3x). The final product (acid) is dried at 80° in a vacuum for 24h, m >300°dec. It contains one mol of water per mol of acid (C30H36N4O13.H2O). The product is pure as revealed... 

The product may be recrystallized from 1 2 acetic acid-water (about 8 ml./g.), but this process effects little improvement in melting point or color, even when activated carbon is used. 

A solution of the crude cyanohydrin (94a ca. 1 g) in pyridine (15 ml) and acetic anhydride (15 ml) is allowed to stand at room temperature for 52 hr. The solvents are evaporated under reduced pressure below 60°. The residue is dissolved in ether, and the ether solution is washed successively with 5 % hydrochloric acid, water and saturated salt solution. The solvent is evaporated under reduced pressure to give a crystalline residue. Recrystallization of the crude product from cyclohexane-acetone gives 3-methoxy-17a-cyano-estra-l,3,5(10)-trien-17i5-ol acetate (94b 0.9 g), mp 130-132°, as large prisms. 

Sorm" " found that when cholesterol acetate (67) is oxidized by chromic acid in acetic acid-water at 55°, crystalline keto seco-acid (69) is obtained in 25-30 % yield from the mother liquors after removal of successive crops of 7-ketocholesterol acetate (68). Reaction of keto acid (69) with benzoyl chloride in pyridine gives a dehydration product, shown" to be the )5-lactone... 

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