Synthesis of Phenol by Partial-Pressure Evaporation

THE present review covers contributions to the art of sulfonation reported in the published literature from about 1941 to the forepart of 1947. In general, this review embraces material reported in Chemical Abstracts as well as information about sulfonation processes used in Germany as described in various government reports-e.g., British Intelligence Objectives Sub-Committee Final Reports (BIOS reports), Field Information Agency Technical Final Reports of the U. S. Government (FIAT reports), and others. The review is limited to INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 40,No. 9 of unreacted oil suitable for recycling. The I.G. Farbenindustrie manufactured Mersolates-i.e., mixtures of Ci6 and Ci6 alkyl

Section: Batch Processingmentioning

confidence: 99%

Sulfonation

Lisk¹

1948

“…In the latter case, where the water formed during a reaction affects the rate, chemical dehydrating agents have been used. An example is sulfuric acid in nitration and sulfonation reactions; it has been proposed (4,6,7) to use the partial-pressure method for the removal of this water produced in both the sulfonation and nitration of benzene.…”

Section: Sulfonation Of Naphthalenementioning

confidence: 99%

Sulfonation of Naphthalene

Othmer¹,

Jacobs²,

Buschmann³

1943

Self Cite

The equipment for this conversion consisted of a concrete mixer, two large wooden tanks, and necessary pump, steam, and water lines. It was assembled as shown in Figure 2. A charge of 200 pounds of ore (ground to 200 mesh), 40 pounds of sodium carbonate (a 25 per cent excess), and 15 gallons of hot water were placed in the concrete mixer. A temperature of about 90°C. was maintained by blowing live steam into the slurry in the mixer during operation. The mixer was allowed to rotate for one hour, and the course of the reaction followed by determining the residue insoluble in dilute hydrochloric acid (Figure 3).Further operations were limited to a 30-minute period of agitation, after which the charge was dumped into a 350gallon tank. One day's operation of 1400 to 1600 pounds of ore about filled the tank. After standing overnight to settle, the clear liquor on top was pumped off, more water added, and the slurry pumped to a 400-gallon tank. This was worked twice by decantation in 24 hours, and the thick slurry taken to a plate dryer. Less than one per cent of water-soluble material remained in the dried product. AcknowledgmentThe pilot-plant experiments were carried out by Edward Ammer of the Manufacturers Mineral Company of Seattle.

“…Othmer and Leyes (20). Certain advantages of speed of reaction, due to the higher operating temperature possible at atmospheric pressure, to the control of the reaction, and to the purity of product due to absence of sulfone formation, have been indicated.…”

Section: Use Of Partial Pressures In Chemical Reactionsmentioning

confidence: 99%

Partial Pressure Processes

Othmer¹

1941

Self Cite

Partial pressure distillation", "stum distilbtion", and "azeotropic distillation" an t e r n used to repment the phenomenon of additive partial pressures due to the mutual immiscibility of many pain of liquids, as well as the methodc of carrying out separating operations and chemical reactions involving one or both of the liquids of the pair. The applications to industrial process are numerous, and tremendous tonnages of materials are separated or manufactured in many different industries by some of the methods described above, othen of the processes or operations described hwe been worked only on a small scale. 1106 swtmba, 1s41 I N D U S T R I A L A N D E N GAPORliquid equilibrium relations can be predicted V for only +ma of pairs of liqui-. e., thoae which sua p e r f d y immisdble and t h w which are perfectly raincible.In the hit oam the individual vapor pmsmrea of the respective matetiah am additive; in every other case more complicated reJations are involved. Thus, the compdtion of the vapm may be found from the law of additive vapor pressurea, which stgtee that the ratio of the molar percentages of the two constituene in the vapor is the same aa the ratio of the individual partial pressures at that temperature. Pok mbly a more convenient way of e x p m thie relation is to h t e that the hiling point of the mixture may be found by plotting the individual vapor pressures on the ordinata of merent temperatures, graphi~dy adding these pressures on these ordinaten, and debmining the intersection of the latter m e with the absciem repwenting the desired operating pmure. If, for example, 760 mm. is the pressure at whiah the b o i i temperatwe is desired, the intersection of the 760 nun. line with the additive curve wiU give the boiling temperature of a mixture of the liquids or the wcalled azstropic point. TaLing, for example, b e n e and water aa the insoluble liquids, the b o i i point of the first is 80.Zo and of the second, 100° C., and the hiling point or place at which the pressure of the combination rescbes 760 mm. is 89.26' C., with 8.83 per cent water and 91.17 per cent bemsene. Thus, the efiective boiling point of water has been reduced to 69.?Ba8" C. when in the presence of bemne. A deecription of a new method of plotting and calculating t h m relations waa recently pre m t e d (17). This addition of the pressures of immiscible liquids is tsken advantage of in industrial opemtions, often 8 p O h of 88 aseotropic distillation, partial pressure distillation, or steam distillation. h m DWiUdion practice of ehnl distillation wbich is used d y for loweringThe most cornmoll u~e of partial pressura distillstionis the the &&ve boiling point of one compound. In thin case the othw compormd is ahno& water, added as steam, and it wrvm to bringover ahigher boillng material at Bmne temperature below the boiling point of water.