Wash recovery, solvent

The technique for the removal of solids by filtration with suction has already been described (Section 2.19). The same technique will of course be applied to the collection of recrystallised compounds. Additionally, however, it should be noted that the mother-liquor from a recrystallisation is often of value for the recovery of further quantities of product, and should be transferred to another vessel after the crystals have been drained and washed with solvent. The mother-liquor may be then subsequently concentrated (Section 2.24 suitable precautions being taken, of course, if the solvent is flammable), and a further crop of crystals obtained. Occasionally yet another crop may be produced. The crops thus isolated are generally less pure than the first crystals which separate, and they should be combined and recrystallised from fresh solvent the purity is checked by a melting point determination. 

Futhermore, difficulty is encountered with many specimens received for examination either because of the absence of accelerant or because of the type of material itself. Examples are (a) heavily charred wood, where all flammable accelerant has been lost, (b) a rag that was soaked in the water used by the fire department to extinguish the blaze, dried out, and forwarded to the forensic chemist for examination and (c) a sample of soap recovered near the site or origin. Analysis of the soap for an accelerant would exclude the solvent wash recovery method as well as any other method that might cause interference due to foaming. 

The compound-nch sorbent should be placed in a sintered glass funnel (3 porosity frit) attached to a glass Buchner flask to which a vacuum is applied. The sorbent is then washed with solvent, and the resulting solution can be recovered in the flask and evaporated to yield the product. Repeated washings with solvent will lead to effective recovery of compounds. This is the method of choice for recovery of components from preparative TLC plates. 

Recently, solid phase extraction (SPE) on several stationary phases has been extensively used in the pretreatment of both plant and biological samples. Typically, crude extracts are mixed with appropriate solvents (methanol or ethanol) and the resulting solutions are applied onto the SPE cartridges. The cartridges are next washed with appropriate solvents to take out impurities and, finally, the taxanes are eluted in an optimized recovery solvent. The obtained taxane fraction is evaporated to dryness and, after reconstimtion to solution, an aliquot is analyzed by HPLC. 

Recovery of sorbed heavy oil from carbon materials was carried out either by filtering under suction (about 5 to 7 kPa pressure), washing with solvents, centrifuging at 3800 rpm, or by squeezing mechanically. The recovered sorbent was repeatedly subjected to sorption of the heavy oil. To determine its cycling performance, this cycle of sorption and recovery (desorption) was repeated up... 

Other Organic Processes. Solvent extraction has found appHcation in the coal-tar industry for many years, as for example in the recovery of phenols from coal-tar distillates by washing with caustic soda solution. Solvent extraction of fatty and resimic acid from tall oil has been reported (250). Dissociation extraction is used to separate y -cresol fromT -cresol (251) and 2,4-x5lenol from 2,5-x5lenol (252). Solvent extraction can play a role in the direct manufacture of chemicals from coal (253) (see Eeedstocks, coal chemicals). 

The Courtaulds semicommercial production system is iUustrated in Figure 8. Dissolving-grade woodpulp is mixed into a paste with NMMO and passes through a high temperature dissolving unit to yield a clear viscous solution. This is filtered and spun into dilute NMMO whereupon the ceUulose fibers precipitate. These are washed and dried, and finally baled as staple or tow products as required by the market. The spin bath and wash Uquors are passed to solvent recovery systems which concentrate the NMMO to the level required for reuse in dissolution. 

The filter cake can then be washed either by displacement or by reslurrying. Reslurrying is easily accompHshed using the stirring action of the rotor blades when the rotor is lowered into the cake. The cake may also be dried in situ by the passage of hot air through it, or may be steam distilled for the recovery of solvent. 

Eig. 1. The key steps for the Phillips PPS process are (/) production of aqueous sodium sulfide from aqueous sodium hydrogen sulfide (or hydrogen sulfide) and aqueous sodium hydroxide 2) dehydration of the aqueous sodium sulfide and NMP feedstocks 5) polymerization of the dehydrated sulfur source with -dichlorobenzene to yield a slurry of PPS and by-product sodium chloride in the solvent (4) polymer recovery (5) polymer washing for the removal of by-product salt and residual solvent (6) polymer drying (7) optional curing, depending on the appHcation and (< ) packaging. 

Various processes involve acetic acid or hydrocarbons as solvents for either acetylation or washing. Normal operation involves the recovery or recycle of acetic acid, any solvent, and the mother Hquor. Other methods of preparing aspirin, which are not of commercial significance, involve acetyl chloride and saHcyHc acid, saHcyHc acid and acetic anhydride with sulfuric acid as the catalyst, reaction of saHcyHc acid and ketene, and the reaction of sodium saHcylate with acetyl chloride or acetic anhydride. 

In general, the sulfolane extraction unit consists of four basic parts extractor, extractive stripper, extract recovery column, and water—wash tower. The hydrocarbon feed is first contacted with sulfolane in the extractor, where the aromatics and some light nonaromatics dissolve in the sulfolane. The rich solvent then passes to the extractive stripper where the light nonaromatics are stripped. The bottom stream, which consists of sulfolane and aromatic components, and which at this point is essentiaHy free of nonaromatics, enters the recovery column where the aromatics are removed. The sulfolane is returned to the extractor. The non aromatic raffinate obtained initially from the extractor is contacted with water in the wash tower to remove dissolved sulfolane, which is subsequently recovered in the extract recovery column. Benzene and toluene recoveries in the process are routinely greater than 99%, and xylene recoveries exceed 95%. 

The cooled mixture is transferred to a 3-1. separatory funnel, and the ethylene dichloride layer is removed. The aqueous phase is extracted three times with a total of about 500 ml. of ether. The ether and ethylene chloride solutions are combined and washed with three 100-ml. portions of saturated aqueous sodium carbonate solution, which is added cautiously at first to avoid too rapid evolution of carbon dioxide. The non-aqueous solution is then dried over anhydrous sodium carbonate, the solvents are distilled, and the remaining liquid is transferred to a Claisen flask and distilled from an oil bath under reduced pressure (Note 5). The aldehyde boils at 78° at 2 mm. there is very little fore-run and very little residue. The yield of crude 2-pyrrolealdehyde is 85-90 g. (89-95%), as an almost water-white liquid which soon crystallizes. A sample dried on a clay plate melts at 35 0°. The crude product is purified by dissolving in boiling petroleum ether (b.p. 40-60°), in the ratio of 1 g. of crude 2-pyrrolealdehyde to 25 ml. of solvent, and cooling the solution slowly to room temperature, followed by refrigeration for a few hours. The pure aldehyde is obtained from the crude in approximately 85% recovery. The over-all yield from pyrrole is 78-79% of pure 2-pyrrolealdehyde, m.p. 44 5°. 

Tower bottoms-ACN, butadiene, with some butenes and acetylenes - are fed to a recovery/stripping column. The hydrocarbons are taken overhead and then rerun to meet product specifications. The stripping column bottoms, (ACN) is then remrned near the top of the extractive distillation tower. A small slipstream goes to the ACN recovery tower, where solvent is also recovered from the water wash streams. 

The vinyl ether may be further purified by dissolving it in 15 ml of dry ether and adding a solution of 0.25 g of lithium aluminum hydride in 10 ml of dry ether. The mixture is refluxed for 30 minutes, and excess hydride is destroyed by addition of ethyl acetate (1 ml). Ice-cold dilute (0.5 N) sulfuric acid (25 ml) is gradually added to the cooled mixture, the ethereal layer is rapidly separated, the aqueous layer is extracted once with 10 ml of ether, and the combined ethereal solution is washed once with water and dried over potassium carbonate. Removal of the solvent, followed by distillation of the residue affords about 85% recovery of the pure vinyl ether, bp 102-10376 mm, 1.5045. 

A 100-ml flask is charged with 25 ml of bromine and 10 g of adamantane and heated under reflux for 3 hours. The cooled mixture is dissolved in 100 ml of carbon tetrachloride, and the carbon tetrachloride solution is washed with 100-ml portions of saturated bisulfite solution until the color of bromine is discharged. The solution is then washed twice with water and dried (magnesium sulfate). The solvent is removed (rotary evaporator) and the product is recrystallized from methanol. (For best recovery of the recrystallized material, the methanol solution should be cooled in a Dry Ice cooling bath.) The product has mp 108°. 

Since no special ligand design is usually required to dissolve transition metal complexes in ionic liquids, the application of ionic ligands can be an extremely useful tool with which to immobilize the catalyst in the ionic medium. In applications in which the ionic catalyst layer is intensively extracted with a non-miscible solvent (i.e., under the conditions of biphasic catalysis or during product recovery by extraction) it is important to ensure that the amount of catalyst washed from the ionic liquid is extremely low. Full immobilization of the (often quite expensive) transition metal catalyst, combined with the possibility of recycling it, is usually a crucial criterion for the large-scale use of homogeneous catalysis (for more details see Section 5.3.5). 

Dissolution/reprecipitation processes were evaluated for the recycling of poly-epsilon-caprolactam (PA6) and polyhexamethyleneadipamide (PA66). The process involved solution of the polyamide in an appropriate solvent, precipitation by the addition of a non-solvent, and recovery of the polymer by washing and drying. Dimethylsulphoxide was used as the solvent for PA6, and formic acid for PA66, and methylethylketone was used as the non-solvent for both polymers. The recycled polymers were evaluated by determination of molecular weight, crystallinity and grain size. Excellent recoveries were achieved, with no deterioration in the polymer properties. 33 refs. 

The stopping solution composition was based on experiments showing that lowering the pH from 9 to 5 to 1 reduced formation of cis-DMNM, perhaps because this prevented elution of the amine from the column, and that addition of ammonium sulfamate lowered cis-DMNM formation, relative to the situation where ascorbate alone was used as a nitrite trap. The hexane wash of the column was introduced to remove a large peak near the solvent front in the GC-TEA, perhaps due to neutral fats. Using the described procedure, the recovery of 70-160 ng NMOR added to 2 g semisynthetic diet was 92 + 19% (mean + S.D. for 13 measurements). The recovery of 227 ng NMOR from 5-8 g whole mouse homogenate using the Iqbal method was 101 + 57% for 7 measurements. 

However, complete hydrolysis of carotenoid esters sometimes is not achieved in 1 to 3 hr. The saponification degree can be verified easily by the presence of carotenol ester peaks eluting later than the peaks of P-carotene on reversed phase columns. Retinol palmitate, added as an internal standard to orange juice, also serves to indicate whether saponification is complete, since it is converted to retinol which elutes at lower retention time. The mixture is subsequently washed with water until free of alkali in a separatory funnel. Other more polar solvents such as CH2CI2 or EtOAc, and diethyl ether alone or mixtured with petroleum ether can be used to increase the recovery of polar xanthophylls from the water phase. 

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