Continuous product extraction

Figure 5.4-3 shows the results of a lifetime study for Wilke s catalyst dissolved, activated, and immobilized in the [EMIM][(CF3S02)2N]/compressed CO2 system. Over a period of more than 61 h, the active catalyst showed remarkably stable activity while the enantioselectivity dropped only slightly. These results clearly indicate - at least for the hydrovinylation of styrene with Wilke s catalyst - that an ionic liquid catalyst solution can show excellent catalytic performance in continuous product extraction with compressed CO2. 

It is noteworthy that, while cells are capable of recovering metal directly, few can achieve continuous product extraction. Other cells are only capable of concentrating the dissolved metal a deposition cycle is necessarily followed by chemical (or anodic) dissolution of the deposit in a small volume of a suitable leaching liquor. 

Degradation with loss of 2 C-atoms—Continuous product extraction s. 12,354... 

With reversible reactions, recycling is warranted when improvement in conversion can be realized by removing some of the product in a separator and returning only unconverted material. In some CSTR operations, the product is removed continuously by extraction or azeotropic distillation. The gasoline addi-... 

Extraction from Aqueous Solutions Critical Fluid Technologies, Inc. has developed a continuous countercurrent extraction process based on a 0.5-oy 10-m column to extract residual organic solvents such as trichloroethylene, methylene chloride, benzene, and chloroform from industrial wastewater streams. Typical solvents include supercritical CO9 and near-critical propane. The economics of these processes are largely driven by the hydrophihcity of the product, which has a large influence on the distribution coefficient. For example, at 16°C, the partition coefficient between liquid CO9 and water is 0.4 for methanol, 1.8 for /i-butanol, and 31 for /i-heptanol. 

Stuckey, D.C., Caridis, K.A., Leak, D.J., Design of a novel bioreactor with cell recycle for continuous biotransformation and product extraction, Proc. 3rd Asia Pacific Biochemical Eng. Conf, Singapore, pp.315-317, 1994. 

A suspension of lithium aluminum deuteride (1.6 g) in dry tetrahydrofuran (60 ml) is added dropwise to a stirred and cooled (with ice-salt bath) solution of 5a-androst-l4-ene-3j3,17j3-diol (179, 1.6 g) and boron trifluoride-etherate (13.3 g) in dry tetrahydrofuran (60 ml). The addition is carried out in a dry nitrogen atmosphere, over a period of 30 min. After an additional 30 min of cooling the stirring is continued at room temperature for 2 hr. The cooling is resumed in a dry ice-acetone bath and the excess deuteriodiborane is destroyed by the cautious addition of propionic acid. The tetrahydrofuran is then evaporated and the residue is dissolved in propionic acid and heated under reflux in a nitrogen atmosphere for 8 hr. After cooling, water is added and the product extracted with ether. The ether... 

Figure 2.5 Possible technological solutions to bioprocess problems a) Fed-batch culture b) Continuous product removal (eg dialysis, vacuum fermentation, solvent extraction, ion exchange etc) c) Two-phase system combined with extractive fermentation (liquid-impelled loop reactor) d) Continuous culture, internal multi-stage reactor e) Continuous culture, dual-stream multi-stage reactor f) Continuous culture with biomass feedback (cell recycling). (See text for further details).

The alternative is hexane, which because of the explosion hazard requires a more expensive type of extractor construction. After the extraction the product is dull gray. The continuos sheet is slit to the final width according to customer requirements, searched by fully automatic detectors for any pinholes, wound into rolls of about 1 m diameter (corresponding to a length of 900-1000 m), and packed for shipping. Such a continuous production process is excellently suited for supervision by modern quality assurance systems, such as statistical process control (SPC). Figures 7-9 give a schematic picture of the production process for microporous polyethylene separators. 

Since 1978, several papers have examined the potential of using immobilised cells in fuel production. Microbial cells are used advantageously for industrial purposes, such as Escherichia coli for the continuous production of L-aspartic acid from ammonium fur-marate.5,6 Enzymes from microorganisms are classified as extracellular and intracellular. If whole microbial cells can be immobilised directly, procedures for extraction and purification can be omitted and the loss of intracellular enzyme activity can be kept to a minimum. Whole cells are used as a solid catalyst when they are immobilised onto a solid support. 

The product workup consisted of continuously extracting the filter cake with tetrahydrofuran (THF) and combining the THF and filtrate to make up a sample for distillation. In some experiments the THF extracted filter cake was extracted with pyridine and the pyridine extract was included in the liquid products. Extraction with pyridine increased coal conversion to soluble products by an average of 1.6 weight percent. The hot filtrate-THF-pyridine extract was distilled. Distillation cuts were made to give the following fractions, THF (b.p. <100 C), light oil (b.p. 100-232 C), solvent (b.p. 232-482), and SRC (distillation residue, b.p. >482 C). 

Straightforward. We have therefore employed XAD-4 to combine biocatalytic synthesis with simultaneous product extraction. The system (Figure 15.8) comprises a continuously stirred tank reactor, a starting material feed pump, a product recovery loop with a (semi-) fluidized bed of XAD-4, and a pump to circulate the entire reaction mixture through the loop." ° Preliminary studies indicated that XAD-4 had no detrimental effects on E. coli JMlOl (pHBP461), hence, separation of biomass and reaction liquid prior to catechol extraction was not required. The biocatalytic reaction was carried out at very low concentrations of the toxic substrate and product. This was achieved by feeding the substrate at a rate lower than the potential bioconversion rate in the reactor. 

Pilot plant operations, as we have noted previously, can vary between extremes of flow rates. It is necessary, therefore, that the feed and reagent volumes be large enough that the pilot plant may be operated for a sufficient length of time to obtain meaningful data. For example, if the aqueous feed to the solvent extraction (SX) circuit is being produced batchwise, variations between batches are bound to occur. Such variations should be controlled as much as possible. Batchwise production of the feed solution may be very different from feed to the actual plant, especially if the plant process involves continuous production of the feed to the SX circuit. 

Concurrently, the butyltellurenyl bromide was obtained by the addition of a solution of bromine (0.16 g, 2.0 mmol) in benzene ( 10 mL) to the solution of dibutylditelluride (0.738 g, 2.0 mmol) in hexane cooled at 0°C under a nitrogen atmosphere. The mixture was stirred at 0°C for 10 min, then LiCl (0.196 g, 4.2 mmol) was added, the dark solution turned clear red and stirring was continued until LiCl was dissolved (10 min). The resulting solution was transferred to the flask containing the vinyl alane. The reaction was stirred for 2 h at room temperature and then a mixture of ice and water ( 60 mL) was added. The solids were filtered and the products extracted with hexane (3X70 mL) and ethyl acetate... 

Reaction of Acetoin (3-Hydroxy-2-butanone) with Ammonia. Aqueous solution of ammonium hydroxyde (20%, 100 ml) was added to acetoin (17.6 g, 0.2 mol) and the reaction mixture was stirred for 30 min at 50°C and then for 6 h at room temperature. The precipitated product was filtered off, the filtrate was neutralized with 10% hydrochloric acid, and extracted with ether (continuous overnight extraction). The extract was washed with water, dried over anhydrous sodium sulfate, and concentrated on a spinning-band distillation apparatus. The residual solution was then analyzed by GC and GC-MS. 

Cognate preparation. 3-Aminopyridine. Prepare a cold sodium hypobromite solution from 32 g (10 ml, 0.2 mol) of bromine and 25 g (0.62 mol) of sodium hydroxide in 250 ml of water. Add in one portion 20 g (0.163 mol) of finely powdered nicotinamide (Expt 6.169) and stir vigorously for 15 minutes. Warm the solution in a water bath at 75 °C for 45 minutes. Isolate the crude product by continuous ether extraction (Section 2.22) of the cooled reaction mixture after saturation with sodium chloride. Dry the extract over potassium hydroxide pellets and remove the ether. Crystallise the dark residue from a 4 1 mixture of benzene-light petroleum (b.p. 60-80 °C) with the aid of decolourising charcoal. The yield of almost colourless product, m.p. 63 °C, is 9.3 g (61%). 

As techniques for chemical analysis are used in continually smaller domains, experimental challenges for inherently insensitive methods such as NMR spectroscopy become increasingly severe. Among the various schemes to boost the intrinsic sensitivity of an NMR experiment, the development of small-volume RF probes has experienced a renaissance during the past decade. Commercial NMR probes now allow analyses of nanomole quantities in microliter volumes from natural product extracts and combinatorial chemical syntheses. Figure 7.3.1.9 illustrates the range of volumes that can be examined by NMR probes and accessories such as microsample tubes and inserts. With recently reported advances in sample preconcentration for microcoil NMR analysis [51], dilute microliter-volume samples can now be concentrated into nanoliter-volume... 

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