With Superheated Steam

The theory of, and the apparatus for, distillation with superheated steam are described in Section 1,7. 

I) The a-naplithylamine may also be isolated directly from the neutralised reaction mixture by distillation with superheated steam (Section 1,6). 

Disposal. Fluorine can be disposed of by conversion to gaseous perfluorocarbons or fluoride salts. Because of the long atmospheric lifetimes of gaseous perfluorocarbons (see Atmospheric models), disposal by conversion to fluoride salts is preferred. The following methods are recommended scmbbing with caustic solutions (115,116) reaction with soHd disposal agents such as alumina, limestone, lime, and soda lime (117,118) and reaction with superheated steam (119). Scmbbing with caustic solution and, for dilute streams, reaction with limestone, are practiced on an industrial scale. 

The unit Kureha operated at Nakoso to process 120,000 metric tons per year of naphtha produces a mix of acetylene and ethylene at a 1 1 ratio. Kureha s development work was directed toward producing ethylene from cmde oil. Their work showed that at extreme operating conditions, 2000°C and short residence time, appreciable acetylene production was possible. In the process, cmde oil or naphtha is sprayed with superheated steam into the specially designed reactor. The steam is superheated to 2000°C in refractory lined, pebble bed regenerative-type heaters. A pair of the heaters are used with countercurrent flows of combustion gas and steam to alternately heat the refractory and produce the superheated steam. In addition to the acetylene and ethylene products, the process produces a variety of by-products including pitch, tars, and oils rich in naphthalene. One of the important attributes of this type of reactor is its abiUty to produce variable quantities of ethylene as a coproduct by dropping the reaction temperature (20—22). 

Fresh reducing gas is generated by reforming natural gas with steam. The natural gas is heated in a recuperator, desulfurized to less than 1 ppm sulfur, mixed with superheated steam, further preheated to 620°C in another recuperator, then reformed in alloy tubes filled with nickel-based catalyst at a temperature of 830°C. The reformed gas is quenched to remove water vapor, mixed with clean recycled top gas from the shaft furnace, reheated to 925°C in an indirect fired heater, and injected into the shaft furnace. For high (above 92%) metallization a CO2 removal unit is added in the top gas recycle line in order to upgrade the quaUty of the recycled top gas and reducing gas. 

S-DlmethyK trattn (2). A mixture of 6,7-dlmethyKetralln 1 (18.0 g, 0.11 mol) and HjSOa was heated under stirring to 80°C and maintained at this temperature for 15 min, then at 25°C for 24 h. The mixture was diluted with water and distilled with superheated steam. From the distillate by extraction with EljO and distillation there was obtained 4.5 g of 2 (24%), bp 110-115°C, no - 1.5530. 

Naphthalene, xylenes and alkyl benzenes can be purified by sulfonation with concentrated sulfuric acid and crystallisation of the sodium sulfonates. The hydrocarbon is distilled out of the mixture with superheated steam. 

Natural gas is desulfurized beeause sulfur has an adverse effeet on the eatalysts used in the reforming and synthesis reaetions. After desulfurization and serubbing, the natural gas is mixed with superheated steam at 23 barg and 510°C. Nitrogen is supplied from the air, whieh is fed to the seeondary reformer at 20 barg and 166°C. Table 5 shows the eomposition of air. 

Glycerol is obtained by the hydrolysis of fats and oils, and purified by distillation under reduced pressure with superheated steam. 

Finally, certain 3-substituted compounds can be prepared by utilizing the - meta) directing powet (cf. Section IV,B) of some groups in the 2-position which afterward can be removed. 3-Nitrothiophene is prepared by nitration of 2-thiophenesulfonyl chloride and by removal of the sulfonic acid group of the 4-nitro-2-sulfonyl chloride formed with superheated steam. Another approach to 3-nitrothio-phene is to nitrate 2-cyanothiophene, separate the 4-nitro-2-cyano-thiophene from the 5-isomer, hydrolyze, and decarboxylate. A final method of preparation of 3-nitrothiophene is by simultaneous de-bromination and decarboxylation of 5-bromo-4-nitro-2-thiophene-carboxylic acid obtained through the nitration of methyl 5-bromo-2-thiophenecarboxylate. 

In the Monsanto/Lummus Crest process (Figure 10-3), fresh ethylbenzene with recycled unconverted ethylbenzene are mixed with superheated steam. The steam acts as a heating medium and as a diluent. The endothermic reaction is carried out in multiple radial bed reactors filled with proprietary catalysts. Radial beds minimize pressure drops across the reactor. A simulation and optimization of styrene plant based on the Lummus Monsanto process has been done by Sundaram et al. Yields could be predicted, and with the help of an optimizer, the best operating conditions can be found. Figure 10-4 shows the effect of steam-to-EB ratio, temperature, and pressure on the equilibrium conversion of ethylbenzene. Alternative routes for producing styrene have been sought. One approach is to dimerize butadiene to 4-vinyl-1-cyclohexene, followed by catalytic dehydrogenation to styrene ... 

A process for depolymerizing nylon-6 and polyester-nylon-6 mixed scrap was patented by Allied Chemical Corporation in 19656 and 1967.7 Ground scrap was dissolved with high-pressure steam at 125-130 psig (963-997 kPa) pressure and 175-180°C for 0.5 h in a batch process and then continuously hydrolyzed with superheated steam at 350°C and 100 psig (790 kPa) to form -caprolactam at an overall recovery efficiency of 98%. The recovered monomer could be repolymerized without additional purification. 

Chemical recycling of nylon-6 carpet face fibers has been developed into a closed-loop recycling process for waste nylon carpet.5 The recovered nylon-6 face fibers are sent to a depolymerization reactor and treated with superheated steam in the presence of a catalyst to produce a distillate containing caprolactam. The crude caprolactam is distilled and repolymerized to form nylon-6. The caprolactam... 

The polycaprolactam waste is contacted with superheated steam in the absence of added catalyst at a temperature of about 250 to 400C and a pressure in the range of about 1.5 to 100 atm. and substantially less than the saturated vapour pressure of water at the temperature at which a caprolactam-containing vapour stream is formed. The resulting caprolactam may then be used in the production of engineered resins and fibres. 

The breaking up of azeotropic mixtures Steam distillation. Distillation of a pair of immiscible liquids Distillation with superheated steam. ... 

Substances which volatilise only with very great difficulty are distilled with superheated steam. The superheating takes place in a copper tube (Fig. 22) wound in a conical spiral, interposed between... 

Figure 16.34. Inversion temperature with superheated steam drying 54)...

Warren Spring describes calibration with methane as a tracer gas. The same holds for cleaning the device. In France it is proposed to clean with superheated steam, followed by a test if every trace of odour is eliminated. 

After heating, the EB is mixed with superheated steam and fed to the first stage reactor. Both the first and second stage reactors are packed with a catalyst of metal oxide deposited on an activated charcoal or alumina pellets. Iron oxide, sometimes combined with chromium oxide or potassium carbonate, is commonly used. 

---