Pilot plant preparation

R.B. Herring, B.L. Beard R. Robbins, The Laboratory and Pilot Plant Preparation of HMX and 75-25 Octol , Holston Defense Corp Report 20-T-14 (1952) 4) O.H. Johnson,... 

Rogers, Pilot Plant Preparation of PBXN-1 By The Stoddard Solvent Slurry Process , NAVORD 5799 (1958). 26) Anon, Thermal And Stability Properties of LASL PBX 9404 , Mason Hanger — Silas Mason Co, Inc, Iowa, nugieS nept a yiyjoj t) n.a. d am bl m,... 

Rogers, Pilot Plant Preparation of PBXN-1 By The Stoddard Solvent Slurry Process , NAVORD 5799 (1958) 26) Anon, Thermal... 

The large-scale pilot plant preparation of the chiral aminochroman antidepressant ebaizotan (also known as NAE-086) was developed by H.J. Federsel and co-workers. The structural features of the target included a disubstituted chroman skeleton, a stereocenter, as well as a non-symmetrical tertiary amine moiety at the C3 position and a secondary carboxamide group at C5. The backbone of the target molecule was constructed using the Perkin condensation of 2-hydroxy-6-methoxybenzaldehyde with hippuric acid under mild conditions. 

Jet Fuels. Product JP-5, before and after acid treating is compared to pilot plant prepared material in Table V. Again both stocks have similar nitrogen, hydrogen and aromatic content. 

In summary, a highly convergent, practical and efficient synthesis of the selective estrogen receptor modulator SERM 2 is now available that is suitable for pilot plant preparation. Key to the success of the process is the generation of 6-methoxy-2-tetralone. The developed laboratory synthesis is a seven step process with an overall yield of >27%. 

W. H. Cauu, Pilot Plant Preparation of Thorium Oxide. USAEC Report CF-.56-1-50, 1956 see also in Homogeneous Reactor Project Quarterly Progress Report for the Period Ending July 31, 1965, US.5.EC Report ORNL-1943, Oak Ridg( National Laboratory, 1955. (p. 198)... 

Pilot plant preparation using industrial equipment is a necessary intermediate step required for a su-cessfull scale-up of the process. It offers the following assets. 

Figure 7 - ComparisaD between labwatory and pilot plant preparation...

History. Methods for the fractionation of plasma were developed as a contribution to the U.S. war effort in the 1940s (2). Following pubHcation of a seminal treatise on the physical chemistry of proteins (3), a research group was estabUshed which was subsequendy commissioned to develop a blood volume expander for the treatment of military casualties. Process methods were developed for the preparation of a stable, physiologically acceptable solution of alburnin [103218-45-7] the principal osmotic protein in blood. Eady preparations, derived from equine and bovine plasma, caused allergic reactions when tested in humans and were replaced by products obtained from human plasma (4). Process studies were stiU being carried out in the pilot-plant laboratory at Harvard in December 1941 when the small supply of experimental product was mshed to Hawaii to treat casualties at the U.S. naval base at Pead Harbor. On January 5, 1942 the decision was made to embark on large-scale manufacture at a number of U.S. pharmaceutical plants (4,5). 

A rack and frame press uses heavy nylon cloth positioned in a wooden frame inside a rack. A measured amount of apple or other fmit mash is added from a hopper above the frame. The mash is leveled with a hand trowel and the edges of the nylon cloth are folded over the mash to encase it and create a cheese. The frame is removed, and a second rack is placed on top of the first cheese the process is repeated until a stack of cheeses is prepared. A hydrauhc ram then appHes gradually increa sing pressure on the stack and expresses the juice. A high yield of juice (80%) is obtained and no press aid is required. Because this process is labor intensive (17), it is mostly used for small farm and pilot-plant operations. 

The preparation of polynitroparaftins has been reviewed (75). 2,2-Dinitropropane has been produced ia pilot-plant quantities by Hquid-phase nitration starting from either propane or 2-nitropropane (76,77) (see Nitration). 

The resulting titanium nitride forms a sintered mass, which must be subsequently milled to form a powder having a wide size distribution. The powders produced by these routes ate typically 0.5—10 )Tm, with a wide size distribution. Very fine powders (0.005—0.5 -lm) have been prepared at pilot-plant scale... 

Difficulties with the Na—S system arise ia part from the ceramic nature of the alumiaa separator the specific P-alumiaa is expeasive to prepare and the material is brittie and quite fragile. Separator failure is the leading cause of early cell failure. Cell failure may also be related to performance problems caused by polarization at the sodium/soHd electrolyte iaterface. Lastiy, seal leakage can be a determiaant of cycle life. In spite of these problems, however, the safety and rehabiUty of the Na—S system has progressed to the poiat where pilot plant production of these batteries is anticipated for EV and aerospace apphcations. 

Adsorption. Adsorption (qv) is an effective means of lowering the concentration of dissolved organics in effluent. Activated carbon is the most widely used and effective adsorbent for dyes (4) and, it has been extensively studied in the waste treatment of the different classes of dyes, ie, acid, direct, basic, reactive, disperse, etc (5—22). Commercial activated carbon can be prepared from lignite and bituminous coal, wood, pulp mill residue, coconut shell, and blood and have a surface area ranging from 500—1400 m /g (23). The feasibiUty of adsorption on carbon for the removal of dissolved organic pollutants has been demonstrated by adsorption isotherms (24) (see Carbon, activated carbon). Several pilot-plant and commercial-scale systems using activated carbon adsorption columns have been developed (25—27). 

Pilot-plant [Hyde, Miller, Packham, and Richards, J. Am. Water Works A.S.SOC., 69, 369 (1977)] and full-scale [Ward, Water Serv., 81, 499 (1977)] flotation in the preparation of potable water is described. 

In addition to the vinyl polymers reviewed in this and the previous seven chapters many others have been prepared. Few have, however, reached the pilot plant stage of manufacture and none appear, at present, to be of interest as plastics. 

Many other cellulose esters have been prepared in the laboratory and some have reached pilot plant status. Of these the only one believed to be of current importance is cellulose caprate (decoate). According to the literature, degraded... 

As described in U.S. Patent 2,595,605, in a pilot plant tank 225 liters of a medium containing the following ingredients was prepared 2% ammonium sulfate, 0.2% potassium di-... 

Other preparations and isolations. If damp methylenedi(nitroformamide) is allowed to stand for several days, the odor of formic acid is noticed, and MEDINA can be isolated from the residue (Ref 11, p 14). The details of scale-up to 150 lb batches, including exp details and flow sheets, and further scale-up with the aim of prodn of 1000 lbs are given. The report describes a fume-off and fire which occurred during the S3rd run. The cause was attributed to a stuck valve which allowed nitric acid to build up in the reactor (Ref 13, p 57). In Ref 16, p 73 there are cost analysis data for pilot plant and large scale prodn, flow sheet for a proposed coml plant, and material balances. The action of acet anhydr on N,Nf-bis(hydroxy-methyl)MEDlNA regenerates MEDINA (Ref 6) the diNa salt of N. N trinitrotrimethylene-diamine, on warming with me ale, ppts the Na salt of MEDINA... 

Against high levels of computer control Is the pre-batch preparation time required for sequencing, software writing and parameter setting, the full details of the latter of course often not available. This activity Is acceptable as a precursor to full scale production but Is felt restrictive and could Inhibit flexibility In a pilot plant. 

If the product is to be used for pharmaceuticals the GMP rules must be obeyed during plant operation. All chemicals to be tested in clinical studies with humans must be prepared according to GMP. This leads to very detailed documentation since if you haven t documented it, you haven t done it . All procedures for manufacturing and changes in procedures are subject to approval by quality control departments. This decreases the flexibility in process development. Products that are contaminated too much must be reprocessed according to the GMP guidelines. All equipment to be used in the pilot plant must be validated before use. 

Based upon laboratory and mini- or pilot-plant experiments process flow-sheets are prepared that also take environmental and safety aspects into consideration. Studies on these aspects are carried out in parallel with chemistry and engineering research in the form of so-called Integrated Process Development (see Heinzle and Hungerbiihler, 1997). 

Column chromatography (CC) can be used at laboratory, pilot-plant, and commercial-plant scales. Preparative chromatography has been utilized for the purification of many fine and even bulk chemicals. 

This version of the Wadsworth-Emmons reaction has been used in the scaled-up syntheses of drugs and drug-candidate molecules. For example, it is used to prepare a cinnamate ester that is a starting material for pilot plant synthesis of a potential integrin antagonist.263... 

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