Recycle impurity

Refining and Isomerization. Whatever chlorination process is used, the cmde product is separated by distillation. In successive steps, residual butadiene is stripped for recycle, impurities boiling between butadiene (—5° C) and 3,4-dichloto-l-butene [760-23-6] (123°C) are separated and discarded, the 3,4 isomer is produced, and 1,4 isomers (140—150°C) are separated from higher boiling by-products. Distillation is typically carried out continuously at reduced pressure in corrosion-resistant columns. Ferrous materials are avoided because of catalytic effects of dissolved metal as well as unacceptable corrosion rates. Nickel is satisfactory as long as the process streams are kept extremely dry. 

For the most part, the zinc materials recovered from secondary materials such as slab zinc, alloys, dusts, and compounds are comparable in quality to primary products. Zinc in brass is the principal form of secondary recovery, although secondary slab zinc has risen substantially over the last few years because it has been the principal zinc product of electric arc furnace (EAF) dust recycling. Impure zinc oxide products and zinc-bearing slags are sometimes used as trace element additives in fertilizers and animal feeds. About 10% of the domestic requirement for zinc is satisfied by old scrap. 

Figure 13.21 Cost trade-offs for purge losses as reactor conversion and recycle impurity concentration change. (Reproduced from Smith R and Linnhoff B, 1988, Trans IChemE, CHERD, 66 195 by permission of the Institution of Chemical Engineers.)...

Figure 13.23 Optimization of reactor conversion and recycle impurity concentration using a univariate search.

As the reactor conversion and recycle impurity changes in the optimization, the most appropriate separation... 

However, our column is connected via material flow with a reactor. In Chap. 4 we show that reactor control often boils down to two issues (1) managing energy (temperature control) and (2) keeping as constant as possible the composition and flowrate of the total reactor feed stream (fresh feed plus recycle streams). The latter goal implies that it may in fact be desirable to control the composition of the recycle stream. This minimizes the variablity in recycle impurity composition back into the reactor. This recycle composition is dictated by the economic tradeoffs between yield, conversion, energy consumption in the separation section, and reactor size. 

Because untreated ethylene is recycled, impurities may accumulate in the system that may affect the overall production of the primary radicals and the molecular-weight developments of the polyethylene product. Chain transfer agents such as ketones, aldehydes, alcohols, hydrogen, or chlorinated components may be added to narrow molecular-weight distribution. 

Several different specifications in items 2-5 will be used to investigate the effects of product quality, conversion, and recycle impurities on the economically optimal steady-state design. However, these do not affect the general stmcture of the design procedure. 

Feed impurities. So far only cases in which the feed is pure have been considered. An impurity in the feed opens up further options for recycle structures. The first option in Fig. 4.4a shows the impurity... 

The hydrogen in the vapor stream is a reactant and hence should be recycled to the reactor inlet (Fig. 4.8). The methane enters the process as a feed impurity and is also a byproduct from the primary reaction and must be removed from the process. The hydrogen-methane separation is likely to be expensive, but the methane can be removed from the process by means of a purge (see Fig. 4.8). 

One further problem remains. Most of the n-butane impurity which enters with the feed enters the vapor phase in the first separator. Thus the n-butane builds up in the recycle unless a purge is provided (see Fig. 4.13a). Finally, the possibility of a nitrogen recycle should be considered to minimize the use of fresh nitrogen (see Fig. 4.136). 

It also should be noted in Fig. 4.4high concentration, then this reduces the loss of valuable raw materials in the... 

Now there are two global variables in the optimization. These are reactor conversion (as before) but now also the concentration of IMPURITY in the recycle. For each setting of the IMPURITY concentration in the recycle, a set of tradeoffs can be produced analogous to those shown in Figs. 8.3 and 8.4. 

However, the concentration of impurity in the recycle is varied as shown in Fig. 8.5, so each component cost shows a family of curves when plotted against reactor conversion. Reactor cost (capital only) increases as before with increasing conversion (see Fig. 8.5a). Separation and recycle costs decrease as before (see Fig. 8.56). Figure 8.5c shows the cost of the heat exchanger network and utilities to again decrease with increasing conversion. In Fig. 8.5d, the purge... 

Feed purification. Impurities that enter with the feed inevitably cause waste. If feed impurities undergo reaction, then this causes waste from the reactor, as already discussed. If the feed impurity does not undergo reaction, then it can be separated out from the process in a number of ways, as discussed in Sec. 4.1. The greatest source of waste occurs when we choose to use a purge. Impurity builds up in the recycle, and we would like it to build up to a high concentration to minimize waste of feed materials and product in the purge. However, two factors limit the extent to which the feed impurity can be allowed to build up ... 

Although acetic acid and water are not beheved to form an azeotrope, acetic acid is hard to separate from aqueous mixtures. Because a number of common hydrocarbons such as heptane or isooctane form azeotropes with formic acid, one of these hydrocarbons can be added to the reactor oxidate permitting separation of formic acid. Water is decanted in a separator from the condensate. Much greater quantities of formic acid are produced from naphtha than from butane, hence formic acid recovery is more extensive in such plants. Through judicious recycling of the less desirable oxygenates, nearly all major impurities can be oxidized to acetic acid. Final acetic acid purification follows much the same treatments as are used in acetaldehyde oxidation. Acid quahty equivalent to the best analytical grade can be produced in tank car quantities without difficulties. 

When the gas available for regeneration is in short supply, the regeneration steps ate often carried out in a closed loop. This recycle of the bed effluent back to the inlet has the advantage of concentrating the impurity and making it easier to separate by condensation or other recovery means. 

A schematic diagram of a six-vessel UOP Cyclesorb process is shown in Figure 15. The UOP Cyclesorb process has four external streams feed and desorbent enter the process, and extract and raffinate leave the process. In addition, the process has four internal recycles dilute raffinate, impure raffinate, impure extract, and dilute extract. Feed and desorbent are fed to the top of each column, and the extract and raffinate are withdrawn from the bottom of each column in a predeterrnined sequence estabUshed by a switching device, the UOP rotary valve. The flow of the internal recycle streams is from the bottom of a column to the top of the same column in the case of dilute extract and impure raffinate and to the top of the next column in the case of dilute raffinate and impure extract. 

The ion-exclusion process for sucrose purification has been practiced commercially by Firm Sugar (104). This process operates in a cycHc-batch mode and provides a sucrose product that does not contain the highly molassogenic salt impurities and thus can be recycled to the crystallizers for additional sucrose recovery. 

Fig. 16. Two-hquid flotation flow sheet (39). The original ROM is kaolin (white clay) that contains 11% impurity in the form of mica, anatase, and siUca. Treatment produces high purity kaolin and a Ti02-rich fraction. A, Kaolin stockpile D, dispersant (sodium siUcate plus alkah) W, water K, kerosene C, collector (sodium oleate) RK, recycled kerosene S, screen M, inline mixer SPR, separator CFG, centrifuge P, product and T, to waste.

The methyl ethyl ketazine forms an immiscible upper organic layer easily removed by decantation. The lower, aqueous phase, containing acetamide and sodium phosphate, is concentrated to remove water formed in the reaction and is then recycled to the reactor after a purge of water-soluble impurities. Organic by-products are separated from the ketazine layer by distillation. The purified ketazine is then hydrolyzed under pressure (0.2—1.5 MPa (2—15 atm)) to give aqueous hydrazine and methyl ethyl ketone overhead, which is recycled (122). The aqueous hydrazine is concentrated in a final distillation column. 

The typical SEA process uses a manganese catalyst with a potassium promoter (for solubilization) in a batch reactor. A manganese catalyst increases the relative rate of attack on carbonyl intermediates. Low conversions are followed by recovery and recycle of complex intermediate streams. Acid recovery and purification involve extraction with caustic and heat treatment to further decrease small amounts of impurities (particularly carbonyls). The fatty acids are recovered by freeing with sulfuric acid and, hence, sodium sulfate is a by-product. 

Stripping of acetylene from the solvent takes place at atmospheric pressure. Pure acetylene is removed from the side of the stripper light impurities are removed overhead and recycled to the compressor. Higher acetylenes are removed from the side of a vacuum stripper with the acetylene overheads being recycled to the bottom of the acetylene stripper. 

Cmde HCl recovered from production of chlorofluorocarbons by hydrofluorination of chlorocarbons contains unique impurities which can be removed by processes described in References 53—62. CICN—CI2 mixtures generated by reaction of hydrogen cyanide and CI2 during the synthesis of (CICN) can be removed from the by-product HCl, by fractional distillation and recycling (see Cyanides) (59). 

Waste Treatment. Environmental concerns have increased the need to treat Hquid discharges from all types of industrial processes, as well as mnoffs where toxic substances appear as a result of leaks or following solubilization (see Wastes, industrial). One method of treatment consists of an ion-exchange system to remove the objectionable components only. Another involves complete or partial elimination of Hquid discharges by recycling streams within the plant. This method is unacceptable unless a cycHc increase in the impurities is eliminated by removing all constituents prior to recycling. 

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