Solvent purification unit

Figure 1.2 Commercial solvent purification unit Pure-Solv 400 Solvent Purification System (reprinted with permission from Innovative Technology).

Modem commercial wet-acid purification processes (see Fig. 4) are based on solvents such as C to Cg alcohols, ethers, ketones, amines, and phosphate esters (10—12). Organic-phase extraction of phosphoric acid is accompHshed in one or more extraction columns or, less frequently, in a series of countercurrent mixer—settlers. Generally, 60—75% of the feed acid P2 s content is extracted into the organic phase as H PO. The residual phosphoric acid phase (raffinate), containing 25—40% of the original P2O5 value, is typically used for fertilizer manufacture such as triple superphosphate. For this reason, wet-acid purification units are almost always located within or next to fertilizer complexes. 

The product from the final purification unit operation is typically in a liquid fraction containing water, a solvent, or a buffer. Based on the... 

The principal causes of radiolysis in a Purex plant are beta and gamma radiation in the first extracting unit (HA) and alpha radiation from plutonium in the plutonium purification units. Accurate calculation of radiation absorption by solvent is difficult, because it depends on details of the dispersion of aqueous and organic phases and contactor geometry. Blake [Bll] has given equations for estimating solvent radiation absorption when these details are known. 

The membranes used for ethanol purification are also suitable for dehydration of many other organic solvents, including methanol, isopropanol, butanol, methyl ethyl ketone, acetone, and chlorinated solvents. Commercial units use up to 12 stages with reheating between stages, and product water contents lower than 100 ppm can be obtained. 

In addition, synthesis gases must be ftee of solvents used in the gas purification units themselves except if methanol is used as a solvent as it is the case in the Rectisol process, for example. 

For on-site separation/purification of recovered solvent it is necessary to consider the number and complexity of distillations needed to obtain materials which are suitably pure for reuse. Where mixtures must be separated into individual solvents this can require several distillations, particularly where the solvents form azeotropes - this can significantly add to costs. The major costs associated with solvent purification are normally the capital required for distillation columns, energy and the additional staffing needs to oversee the operation. Where azeotropic distillations are required the cost of distillation columns can be greater than the capital cost of the recovery unit itself and staffing costs can be a significant variable cost (particularly if batch distillation is required). 

From a manufacturing standpoint, the interfacial process is capital-intensive to purify the resin solution, isolate and dry the resin, and recycle solvents and brine. With melt transesterification, because it is a solventless process, the only recycle streams that must be dealt with are those related to the recovery of phenol for reuse in the production of DPC. Hence, there is no need to invest in solvent recovery infrastructure with the melt process, and polymer purification units and dryers can likewise be avoided. However, these investments are somewhat diminished by the investment required for the preparation and purification of DPC. 

A typical extractive fermentation process EFP includes a fermentor, the solvent recovery unit, and the product purification unit. The biotransformation reaction is carried out in the aqueous (nutrient) phase, which contains the substrate and the microorganisms. The recovery and purification stages are preferably done via simple distillation, and can be carried out in the same equipment according to the extract mixture. 

After the actual reaction, a separation process to obtain a pol mier of a certain purity and state follows. Usually, thermal and mechanical imit operations are applied. Pol miers may include residual monomer and solvents which are often difficult to remove. Special consideration has to be given to this subject in the polymers industry in a perspective of life-cycle impact of the products. In the context of the IPPC Directive, the focus is on the minimisation of the emissions of monomers at the industrial site [27, TWGComments, 2004]. Separated monomers, mostly as gases, can be directly returned to the process, returned to the monomer unit to be prepared for purification, transmitted to a special purification unit, or flared off Other separated liquids and solids are sent to a centralised clean-up or recycling unit. Additives needed for processing or for protection may be added to the polymer at this point. 

Most by-product acetylene from ethylene production is hydrogenated to ethylene in the course of separation and purification of ethylene. In this process, however, acetylene can be recovered economically by solvent absorption instead of hydrogenation. Commercial recovery processes based on acetone, dimetbylform amide, or /V-metby1pyrro1idinone have a long history of successfiil operation. The difficulty in using this relatively low cost acetylene is that each 450, 000 t/yr world-scale ethylene plant only produces from 7000 9000 t/yr of acetylene. This is a small volume for an economically scaled derivatives unit. 

C. Isolation and purification of XK-62-2 100 g of the white powder obtained in the above step B are placed to form a thin, uniform layer on the upper part of a 5 cm0X 150 cm column packed with about 3 kg of silica gel advancely suspended in a solvent of chloroform, isopropanol and 17% aqueous ammonia (2 1 1 by volume). Thereafter, elution is carried out with the same solvent at a flow rate of about 250 ml/hour. The eluate is separated in 100 ml portions. The active fraction is subjected to paper chromatography to examine the components eluted. XK-62-2 is eluted in fraction Nos. 53-75 and gentamicin Cja is eluted in fraction Nos. 85-120. The fraction Nos. 53-75 are combined and concentrated under reduced pressure to sufficiently remove the solvent. The concentrate Is then dissolved in a small amount of water. After freeze-drying the solution, about 38 g of a purified preparate of XK-62-2 (free base) is obtained. The preparate has an activity of 950 units/mg. Likewise, fraction Nos. 85-120 are combined and concentrated under reduced pressure to sufficiently remove the solvent. The concentrate is then dissolved in a small amount of water. After freeze-drying the solution, about 50 g of a purified preparate of gentamicin Cja (free base) is obtained. 

Unless odierwise specified, all monomers, reactants, and solvents were reagent grade 99+% (from Aldrich or Fluka) and used without further purification. In polymer formulas, n, x, y, and z represent number-average numbers of repeating units. 

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