Additives separators

An additional separator is now required (Fig. 4.2a). Again, the unreacted FEED is normally recycled, but the BYPRODUCT must be removed to maintain the overall material balance. An additional complication now arises with two separators because the separation sequence can be changed (see Fig. 4.26). We shall consider separation sequencing in detail in the next chapter. 

Can the loss of useful material in the purge be avoided or reduced by additional separation on the purge The roles of refrigerated condensation, membranes, etc. in this respect have already been discussed. 

Can the useful material lost in the purge streams be reduced by additional reaction If the purge stream contains significant quantities of reactants, then placing a reactor and additional separation on the purge can sometimes be justified. This technique is used in some designs of ethylene oxide processes. 

Because there is a mixture of FEED, PRODUCT, and BYPRODUCT in the reactor effluent, an additional separator is required. 

Employ additional separation of waste streams to allow increased recovery. 

If waste streams can be recycled directly, this is clearly the simplest method for reducing waste. Most often, though, additional separation is required or a different separation method is needed to reduce waste. 

Additional separation and recycling. Once the possibilities for recycling streams directly, feed purification, and eliminating the use of extraneous materials for separation that cannot be recycled efiiciently have been exhausted, attention is turned to the fourth option, the degree of material recovery from the waste streams that are left. One very important point which should not be forgotten is that once the waste stream is rejected, any valuable material turns into a liability as an effluent material. The level of recovery in such situations needs careful consideration. It may be economical to carry out additional separation of the valuable material with a view to recycling that additional recovered material, particularly when the cost of downstream effluent treatment is taken into consideration. 

Perhaps the most extreme situation is encountered with purge streams. Purges are used to deal with both feed impurities and byproducts of reaction. In the preceding section we considered how the size of purges can be reduced in the case of feed impurities by purifying the feed. However, if it is impractical or uneconomical to reduce the purge by feed purification, or the purge is required to remove a byproduct of reaction, then the additional separation can be considered. 

For a single stage separator i.e. only one separator vessel, there is an optimum pressure which yields the maximum amount of oil and minimises the carry over of heavy components into the gas phase (a phenomenon called stripping). By adding additional separators to the process line the yield of oil can be increased, but with each additional separator the incremental oil yield will decrease. 

The butane-containing streams in petroleum refineries come from a variety of different process units consequently, varying amounts of butanes in mixtures containing other light alkanes and alkenes are obtained. The most common recovery techniques for these streams are lean oil absorption and fractionation. A typical scheme involves feeding the light hydrocarbon stream to an absorber-stripper where methane is separated from the other hydrocarbons. The heavier fraction is then debutanized, depropanized, and de-ethanized by distillation to produce C, C, and C2 streams, respectively. Most often the stream contains butylenes and other unsaturates which must be removed by additional separation techniques if pure butanes are desired. 

Mercurous Nitrate. Mercurous nitrate [10415-75-5] Hg2N20 or Hg2(N02)2, is a white monoclinic crystalline compound that is not very soluble in water but hydrolyzes to form a basic, yellow hydrate. This material is, however, soluble in cold, dilute nitric acid, and a solution is used as starting material for other water-insoluble mercurous salts. Mercurous nitrate is difficult to obtain in the pure state directly because some mercuric nitrate formation is almost unavoidable. When mercury is dissolved in hot dilute nitric acid, technical mercurous nitrate crystallizes on cooling. The use of excess mercury is helpful in reducing mercuric content, but an additional separation step is necessary. More concentrated nitric acid solutions should be avoided because these oxidize the mercurous to mercuric salt. Reagent-grade material is obtained by recrystaUization from dilute nitric acid in the presence of excess mercury. 

Uranium Purification. Subsequent uranium cycles provide additional separation from residual plutonium and fission products, particularly zirconium— niobium and mthenium (30). This is accompHshed by repeating the extraction/stripping cycle. Decontamination factors greater than 10 at losses of less than 0.1 wt % are routinely attainable. However, mthenium can exist in several valence states simultaneously and can form several nitrosyl—nitrate complexes, some for which are extracted readily by TBP. Under certain conditions, the nitrates of zirconium and niobium form soluble compounds or hydrous coUoids that compHcate the Hquid—Hquid extraction. SiUca-gel adsorption or one of the similar Hquid—soHd techniques may also be used to further purify the product streams. 

To reduce catalyst losses even further, additional separation equipment external to the regenerator can be installed. Such equipment includes third-stage cyclones, electrostatic precipitators, and more recentiy the Shell multitube separator, which is Hcensed by the Shell Oil Co., UOP, and the M. W. Kellogg Co. The Shell separator removes an additional 70—80% of the catalyst fines leaving the first two cyclones. Such a third-stage separator essentially removes from the due gas stream all particles greater than 10 p.m (36). 

The simple batch stUl provides only one theoretical plate of separation. Its use is usuaUy restric ted to preliminary work in which products will be held for additional separation at a later time, when most of the volatile component must be removed from the batch before it is processed further, or for simUar uoucritical separations. 

Unless the hquid pool is purposely lengthened vertically in order to give additional separation via bubble fractionation, it is usually taken to represent one theoretical stage. A bubbler submergence or 30 cm or so is usually ample for a solute with a molecular weight that does not exceed several hundred. 

When a mixture of compounds is to be treated, more limitations may be placed upon the selection of a suitable abatement method. There may be several compounds in the waste gas, some being unsuitable to one method, while others are unsuitable to another method. In such cases, thermal incineration may be the best solution. When recovering mixtures, additional separation equipment may be needed for recycling the reclaimed compounds. 

Although on-line sample preparation cannot be regarded as being traditional multidimensional chromatography, the principles of the latter have been employed in the development of many on-line sample preparation techniques, including supercritical fluid extraction (SFE)-GC, SPME, thermal desorption and other on-line extraction methods. As with multidimensional chromatography, the principle is to obtain a portion of the required selectivity by using an additional separation device prior to the main analytical column. 

Of course, homogeneous catalysis of course also has disadvantages. The main problem is the separation of catalyst and product. This is often only feasible for low molecular weight products. The u.se of solvents requires an additional separation step. 

Hence, P-C bond-cleavage followed by isomerization is responsible for the formation of side products. Furthermore, due to destabilization of the catalyst complex, deactivation occurs and palladium black is formed, which is a notorious disadvantage of Pd-phosphine catalysts in general. Catalyst decomposition and the formation of side products causes additional separation and catalyst recovery problems. These problems have been solved by the discovery of novel catalyst complexes, which are active and stable at temperatures of over 250 °C (Cornils and Herrmann, 1996). 

Using MS detection relaxes the constraints on LC resolution, because additional separation occurs in the mass domain. In principle, LC-MS may yield a complete 2D distribution of a polymer according to chemical composition and molar mass. If MS detection is employed, the efficient cleaning in the LC step makes it possible to use total ion monitoring and even to identify unknown compounds from the sample. As extracts often contain interfering compounds, mass spectrometry in selective ion mode is a practical detector. Fully automated multidimensional LC-MS-MS-MS systems are available. 

The best method or the most suitable combination of methods can be discussed only in regard to the actual analytical problem. The ideal method for polymer analysis in an industrial environment is often essentially that practical one which identifies and quantitates the desired components at the lowest acceptable total cost for the customer, compatible with the desired accuracy and time constraints. Three examples may illustrate the necessary pragmatic trade-off. Despite being old methods, classical polymer/additive analysis techniques, based on initial additive separation from the polymer matrix through solvent extraction methods followed by preconcentration, still enjoy great popularity. This... 

Extraneous material can create additional separation problems, requiring new separations that do not exist inherently within the process. 

Consider the example of a process that involves the multiple reactions in Equation 13.3. Because there is a mixture of FEED, PRODUCT and BYPRODUCT in the reactor effluent, an additional separator is required. The economic trade-offs now become more complex and a new cost must be added to the trade-offs. This is a raw materials efficiency cost due to byproduct formation. If the PRODUCT formation is kept constant, despite varying levels of BYPRODUCT formation, then the cost can be defined to be1112 ... 

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