Run a pilot experiment

The first thing to do is to run a pilot experiment and observe all that can be observed  

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When a synthetic procedure is run for the first time at the bench, a satisfactory result is obtained only rarely. If the purpose of the experiment was to prepare a limited quantity, e.g. for spectroscopic characterization or for toxicological screening, it is probably of minor importance if the yield was low. If, on the other hand, the purpose was to check a new method, or to run a pilot experiment for larger-scale preparation, a poor yield is often a starting point for tedious work to develop the procedure. 

D . The reaction is rather slow at room temperature, at least in the second bromination step. Run a pilot experiment to see if the reaction can be kept under control (exothermic ) if the bromine is added rapidly. If the reaction is not exothermic, use rapid addition in all experiments and do not vary D. 

To determine the reproducibility of the experimental procedure, a pilot experiment (T = 25 °C, = 1.2 M) was run five times before the response... 

My own technical experience has pretty much followed this history of distillation simulation. My practical experience started back in a high-school chemistry class in which we performed batch distillations. Next came an exposure to some distillation theory and running a pilot-scale batch distillation column as an undergraduate at Penn State, learning from Arthur Rose and Black Mike Cannon. Then, there were five years of industrial experience in Exxon refineries as a technical service engineer on pipestills, vacuum columns, light-ends units, and alkylation units, all of which used distillation extensively. 

So far, one application of Equations 19 and 21 is demonstrated they can also be used to determine the sample size of an experiment. In this case, the parameters should be assumed unknown, but Equation 21 involves the unknown Weibull modulus w. As a solution, a pilot experiment can be conducted to gain some information about m this is the first stage of the experiment. Using this information, a decision can be reached about the number of additional measurements required in order to satisfy certain precision requirements. In other words, the information from the first stage is used to determine the size of the experiment to be run in the second stage. The two stages constitute the full experiment. 

The ethylbenzene experiments were run by BP in a pilot loop reactor similar to that described for the dimerization (Figure 5.3-8). 

One year later, Burrows published results from a comprehensive series of experiments using 100% Douglas-fir bark as furnish for particleboard (35). No binder was used he relied upon the "self-bonding" properties of Douglas-fir bark. Variables included bark particle size, mat moisture content, pressing pressure, and use of various overlays. Additional boards were made from ponderosa pine, western hemlock, and white fir barks. A pilot-plant-size run was made using results gathered from the study. 

Then, a pilot plant with a capacity of lOt/a was build for the Swern-Moffat oxidation [57,58]. The yield of the batch process is 83% at — 70 °C, whereas the microchemical process achieved a yield of 88% at 20 °C. The pilot plant was operated under stable reaction conditions for a long run with similar product yields as in the laboratory experiment (see Figure 5.23). 

The furnaces obviously constitute the essential equipment of die hot section of the steam-cracking process, and they condition the satisfactory running of the overall installation. However, their optimal operating conditions and the netibility of the process to operating parameters can often only be evaluated on the ccmpletion of full-scale experiments on a pilot furnace. 

After a little experience, the operation of the pilot unit was smooth and easy. In general the operation was stable and easier to control than in a conventional alkylation unit. In one run some water was accidentally introduced into the alkylation system. The system acid rapidly dropped to about 80% titratable acidity without causing a run-away (24), as would have been the case in conventional alkylation. 

Is there evolution of heat It is strongly recommended that the pilot experiment is run with a thermometer inserted in the reaction mixture. Evolvement of heat may indicate that the stirring rate and the efficiency of the temperature control are critical. 

Some data from a pilot plant series covering a wide salinity range, listed in Table III, illustrate the approximate scope of the pilot plant development work. The experiment described is neither one of the most nor of the least successful. The units for the Eilat plant were designed by combining the conclusions from the data of the runs in the Israeli pilot plant with the experience of the American partner in component and process design in other fields of chemical engineering. 

BP Chemicals studied the use of chloroaluminates as acidic catalysts and solvents for aromatic alkylation [43]. At present, the AICI3 existing technology (based on red oil catalyst) is still used industrially, but continues to suffer from poor catalyst separation and recycle [44]. The aim of the work was to evaluate the AlCls-based ionic liquids, with the emphasis placed on the development of a clean and recyclable system for the production of ethylbenzene (benzene/ethene alkylation) and synthetic lubricants (alkylation of benzene with 1-decene). The production of linear alkyl benzene (LAB) has also been developed by Akzo [45]. The eth)4benzene experiments were run by BP in a pilot loop reactor similar to that described for the dimerization (Fig. 5.4-8). 

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