Batch reactors laboratory scale

Apparatus. Since all the polymer modification reactions presented in this paper involved gas consumption, an automated gas consumption measuring system was designed, fabricated and used to keep constant pressure and record continuously the consumption of gas in a batch type laboratory scale reactor. Process control, data acquisition, and analysis was carried out using a personal computer (IBM) and an interface device (Lab-master, Tecmar Inc.). 

Batch vs Continuous Reactors. Usually, continuous reactors yield much lower energy use because of increased opportunities for heat interchange. Sometimes the savings are even greater in downstream separation units than in the reaction step itself Especially for batch reactors, any use of refrigeration to remove heat should be critically reviewed. Batch processes often evolve Httle from the laboratory-scale glassware setups where refrigeration is a convenience. 

Batch reactors often are used to develop continuous processes because of their suitabiUty and convenient use in laboratory experimentation. Industrial practice generally favors processing continuously rather than in single batches, because overall investment and operating costs usually are less. Data obtained in batch reactors, except for very rapid reactions, can be well defined and used to predict performance of larger scale, continuous-flow reactors. Almost all batch reactors are well stirred thus, ideally, compositions are uniform throughout and residence times of all contained reactants are constant. 

On the laboratory scale, it is usually safe to assume that a batch reactor is stirred to uniform composition, but for critical cases such as high viscosities this could be checked with tracer tests. 

As far as industrial applications are concerned, the easy scale-up of two-phase catalysis can be illustrated by the first oxo aqeous biphasic commercial unit with an initial annual capacity of 100,000 tons extrapolated by a factor of 1 24,000 (batch-wise laboratory development production reactor) after a development period of 2 years [4]. 

Most kinetic experiments are run in batch reactors for the simple reason that they are the easiest reactor to operate on a small, laboratory scale. Piston flow reactors are essentially equivalent and are implicitly included in the present treatment. This treatment is confined to constant-density, isothermal reactions, with nonisothermal and other more complicated cases being treated in Section 7.1.4. The batch equation for component A is... 

In this context, the esterification of 4-(l-pyrenyl)butyric acid with an alcohol to the corresponding ester was investigated [171]. Without the presence of sulfuric acid no reaction to the ester was foimd in the micro reactor. On activating the surface by a sulfuric acid/hydrogen peroxide mixture, however, a yield of 9% was achieved after 40 min at 50 °C. On making the surface hydrophobic by exposure to octadecyltrichlorosilane, no product formation was observed. Using silica gel in a laboratory-scale batch experiment resulted in conversion, but substantially lower than in the case of the micro reactor. The yield was no higher than 15% (40 min ... 

There is an additional point to be made about this type of processing. Many gas-phase processes are carried out in a continuous-flow manner on the macro scale, as industrial or laboratory-scale processes. Hence already the conventional processes resemble the flow sheets of micro-reactor processing, i.e. there is similarity between macro and micro processing. This is a fimdamental difference from most liquid-phase reactions that are performed typically batch-wise, e.g. using stirred glass vessels in the laboratory or stirred steel tanks in industrial pilot or production plants. 

GL 23] [R 12] [P 16] Conversions near 70% were determined for a mini trickle-bed reactor (flow rate 20 mg min ) [36]. The corresponding reaction rate was 10 times larger than in typical batch operation on a laboratory-scale, which is restricted to milder conditions. 

FIGURE 15.1 Schematic diagram of a laboratory-scale, sequencing batch (bio) reactor (SBR). 

A continuous MW reactor (CMR), which operates by passing a reaction mixture through a pressurized tubular microwave-transparent coil and a MW batch reactor (MBR), have been developed by CSIRO in Australia and are used for organic synthesis on the laboratory scale [8]. The CMR can be operated at pressures up to 1400 kPa and temperatures up to 200 °C and the MBR at pressures and temperatures up to 10 MPa and 260 °C. 

This procedure was scaled up from 50 mmol to the 2 mol scale (i.e. from 15.6 to 622.4 g total starting materials) in a larger batch reactor (Synthewave 1000) [12]. Yields were equivalent to those obtained under the original conditions (5 min, 160 °C) in the laboratory-scale experiment (Synthewave 402) (Tab. 5.2). 

A complementary, more advanced, laboratory-scale microwave batch reactor for synthesis and kinetics studies was developed by Strauss et al. [113] (Fig. 10.2). 

A batch reactor (BR) is sometimes used for investigation of the kinetics of a chemical reaction in the laboratory, and also for larger-scale (commercial) operations in which a number of different products are made by different reactions on an intermittent... 

While batch reactors remain the workhorse in fine chemical production, the need to switch to continuous processes will increase the use of meso- and micro-structured reactors both at the laboratory scale (for discovery, process data determination, demonstration, small-scale production) and at the production level. 

The RC1 is an automated laboratory batch/semi-batch reactor for calorimetric studies which has proven precision. The calorimetric principle used and the physical design of the system are sound. The application of the RC1 extends from process safety assessments including calorimetric measurements, to chemical research, to process development, and to optimization. The ability of the RC1 to generate accurate and reproducible data under simulated plant scale operating conditions may result in considerably reduced testing time and fewer small scale pilot plant runs. 

Figure 6.7 A typical batch reactor used for small-scale laboratory reactions. The view through the cell is shown (a) together with the dismantled cell (b) Here, the screw thread which holds the window in place can be seen, along with the sapphire window. The holes on top of the cell allow it to be connected to the high-pressure system with the relevant adaptors. (Photograph by Dr A. P. Abbott)...

Chabot s work was done in a laboratory-scale batch reactor. Experiments at lab scale are a common hrst step in process analyzer work, since they allow technical feasibility to be demonstrated relatively quickly and inexpensively without having to interfere with production targets in a commercial-scale plant. In this work, moreover, one of the two business goals (improving process understanding) could be largely accomplished without going beyond lab-scale experimentation. 

The experimental batch reactor is usually operated isothermally and at constant volume because it is easy to interpret the results of such runs. This reactor is a relatively simple device adaptable to small-scale laboratory set-ups, and it needs but little auxiliary equipment or instrumentation. Thus, it is used whenever possible for obtaining homogeneous kinetic data. This chapter deals with the batch reactor. 

Small steady-state reactors are fiequently the next stage of scaleup of a process from batch scale to full commercial scale. Consequently, it is common to follow batch experiments in the laboratory with a laboratory-scale continuous-reactor process. This permits one both to improve on batch kinetic data and simultaneously to examine more properties of the reaction system that are involved in scaling it up to commercial size. Continuous processes almost by definition use much more reactants because they run continuously. One quickly goes from small bottles of reactants to barrels in switching to... 

Industrially relevant consecutive-competitive reaction schemes on metal catalysts were considered hydrogenation of citral, xylose and lactose. The first case study is relevant for perfumery industry, while the latter ones are used for the production of sweeteners. The catalysts deactivate during the process. The yields of the desired products are steered by mass transfer conditions and the concentration fronts move inside the particles due to catalyst deactivation. The reaction-deactivation-diffusion model was solved and the model was used to predict the behaviours of semi-batch reactors. Depending on the hydrogen concentration level on the catalyst surface, the product distribution can be steered towards isomerization or hydrogenation products. The tool developed in this work can be used for simulation and optimization of stirred tanks in laboratory and industrial scale. 

Any reaction exhibiting substrate inhibition should not be carried out in batch since it results in a longer residence time the high concentration of the substrate at the beginning lowers the reaction rate. A continuously operated stirred tank is preferred. At laboratory scale, fed-batch operation enables a low substrate concentration in the reactor and a higher reaction rate. 

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