Process pilot-scale

Particular attention should be paid to nonstandard production technologies including nonstandard methods of sterilization, sterile filtration and aseptic processing, lyophilization, microencapsulation, and certain critical mixing and coating operations. With such processes pilot-scale manufacture may not be predictive of industrial scale manufacture, and data on three full-scale production batches may be required in the application. 

Chematur AquaCritox process (pilot scale) Sweden N-containing wastes, 250kgh 1998... 

The USD A Flax Pilot Plant (Flax-PP) contains a separate research component for enzyme-retting plant stalks to engineer fibers with desired properties, to optimize enzyme-retting, and to enhance processing. Pilot scale tests of commercially cleaned flax indicated that fiber strength, fineness, and yield could be varied by enzyme/chelator levels (Akin et al. 2001). Our proposed current method to enzymatically ret flax stalks includes commercial pectate lyases after chelator for high... 

Downing, L. S., Bibby, K. J., Esposito, K., Fascianella, T, Tsuchihashi, R. and Nerenberg, R. 2010. Nitrogen Removal from Wastewater Using a Hybrid Membrane-Bioflhn Process Pilot-Scale Studies. Water Environment Research, 82,195-201. 

Fig. 7.3 Scheme of continuously working PGSS process (pilot scale)... 

Under constant pattern conditions the LUB is independent of column length although, of course, it depends on other process variables. The procedure is therefore to determine the LUB in a small laboratory or pilot-scale column packed with the same adsorbent and operated under the same flow conditions. The length of column needed can then be found simply by adding the LUB to the length calculated from equiUbrium considerations, assuming a shock concentration front. 

Another important class of titanates that can be produced by hydrothermal synthesis processes are those in the lead zirconate—lead titanate (PZT) family. These piezoelectric materials are widely used in manufacture of ultrasonic transducers, sensors, and minia ture actuators. The electrical properties of these materials are derived from the formation of a homogeneous soHd solution of the oxide end members. The process consists of preparing a coprecipitated titanium—zirconium hydroxide gel. The gel reacts with lead oxide in water to form crystalline PZT particles having an average size of about 1 ]lni (Eig. 3b). A process has been developed at BatteUe (Columbus, Ohio) to the pilot-scale level (5-kg/h). 

Titanium disulfide can also be made by pyrolysis of titanium trisulfide at 550°C. A continuous process based on the reaction between titanium tetrachloride vapor and dry, oxygen-free hydrogen sulfide has been developed at pilot scale (173). The preheated reactants ate fed iato a tubular reactor at approximately 500°C. The product particles comprise orthogonally intersecting hexagonal plates or plate segments and have a relatively high surface area (>4 /g), quite different from the flat platelets produced from the reaction between titanium metal and sulfur vapor. The powder, reported to be stable to... 

Mobil Oil Corporation has developed a process on a pilot scale that can successfully convert methanol into 96 octane gasoline. Although methanol can be used directiy as a transportation fuel, conversion to gasoline would eliminate the need to modify engines and would also eliminate some of the problems encountered using gasoline—methanol blends (see Alcohol fuels Gasoline and other motor fuels). 

Brassylic Acid. This acid is commercially available from Nippon Mining Company (Tokyo, Japan). It is made by a fermentation process (76). Several years ago, Emery Group, Henkel Corp. (Cincinnati, Ohio) produced brassyUc acid via ozonization of emcic acid primarily for captive use in making dimethyl brassylate and ethylene brassylate. A pilot-scale preparation based on ozonization of emcic acid has been described in which brassyUc acid yields of 72—82% were obtained in purities of 92—95%. Recrystallization from toluene gave purities of 99% (77). 

Application equipment. Laboratory or pilot scale equipment that closely simulates the actual bonding process under production conditions. For some applications this is simple table top equipment, while for others this may be an expensive pilot line with a skilled operator. 

Chemical Flowsheet Basic unit operation selection with flow rates, conversion factors, temperatures, pressures, solvents and catalyst selection Process synthesis route Laboratory and pilot scale trials Knowledge of existing processes... 

The guidance document requires calculation of actual yields and percentages of expected yields. The yield should be recorded at the conclusion of each phase of manufacturing of an API. The expected yield and ranges are established during process validation or from a pilot-scale production run [66]. 

You are now familiar with the major characteristics of organisms that are useful for SCP production, and the types of substrates on which they can be grown. We are now going to consider in detail the processes that have been developed. Some of these processes have been developed only as far as the pilot scale, and have not reached commercial operation. Others have reached full production scale but have subsequently failed, for a variety of reasons. These have been included as well as the successes, as they show you the variety in the technology of SCP production, and also show how economic and political factors influence the success and failure of processes. These processes might also become useful and economic some time in the future. Emphasis will be put on the technology involved in the fermentation and down-stream processing of each process. 

Processes have been developed in North America to pilot scale growing the bacterium Cellulomonas or the fungus Trichoderma on pre-treated milled cellulosic material in conventional fermentors, ie in a liquid medium. However, preparation costs are considerably higher than with solid-substrate fermentations. 

As stated above under TNMe, in Ger during WWII, the prepn of TeNMe by this process was scaled up for use as an intermediate and as a substitute for nitric acid in the V-2 rocket (Ref 26). A pilot plant was built at Newark, NJ for prodn using this procedure. It was destroyed by an expln in 1953 and not rebuilt (Refs 33 44). Other prepns of lesser importance are by the action of Ag nitrite on iodotrinitro-methane (Ref 3) by the action of 90% nitric acid and 25% oleum on malononitrile, yield 45% (Ref 40) by the action of mixed acid on a number of aromatic nitrocompounds, of which nitrobenzene, dinitrobenzene, and nitronaphtha-lene gave the best yields (Ref 13a) and by the action of nitryl chloride on salts of TNMe. 

Farley and Ray (F3) have reported holdup and conversion data for the Fischer-Tropsch process carried out in a pilot-scale reactor. 

Kolbel et al. (K16) examined the conversion of carbon monoxide and hydrogen to methane catalyzed by a nickel-magnesium oxide catalyst suspended in a paraffinic hydrocarbon, as well as the oxidation of carbon monoxide catalyzed by a manganese-cupric oxide catalyst suspended in a silicone oil. The results are interpreted in terms of the theoretical model referred to in Section IV,B, in which gas-liquid mass transfer and chemical reaction are assumed to be rate-determining process steps. Conversion data for technical and pilot-scale reactors are also presented. 

As an example for continuous process design, 2-keto-3-deoxy-D lycero-D-galacto-nonosouate (KDN) (S) has been produced on a 100-g scale from D-mannose and pyruvate using a pilot-scale EMR at a space-time yield of 375 gl d and an overall crystallized yield of 75% (Figure 10.6) [47]. Similarly, L-KDO (6) can be synthesized from L-arabinose [48]. 

The input of the process is a separately collected PVC fraction. The quality has to be about similar as for PVC bound for mechanical recycling. The pilot scale tests... 

During the development phase a series of laboratory or pilot-scale batches will be subjected to this stability program. As soon as the process is scaled up to production-size batches, the first few, and at least one per year thereafter will also go on stability. Submission is only possible if the product completes a minimal combination of tests, e.g., one full-size batch for 12 months and two reduced-size batches for 6 months... 

---