Funnel pressure reactor

Figure 1. Photograph of addition funnel pressure reactor (left) and simple pressure reactor (right). The pressure vessel and associated couplings are omitted from the addition funnel design for clarity.

Figure 3. Expanded view of pressure—equalizing addition funnel pressure reactor. The glass vessel and associated couplings are omitted for clarity. The Teflon tubing is shown as the cross-hatched tubing at lower right, while the stainless steel tubing is depicted at left. (Component illustrations reproduced with permission of Swagelok Company).

Addition funnel pressure reactor, 201 Adjustable pressure relief valve, 200 Aerial oxidation, 64 Aerobic product transfer, 193 Aerosol pressure vessel, 198 Air-sensitive materials decomposition, 147 HPLC analysis, 24 recovering, 193 synthesis and handling, 34 Alkyne electron density, 287 Alkyne ligand, 282 Alkyne it donor orbitals, 287 Alkyne levels, 285 Ambient pressure flow cell, 238-244 Ammonia synthesis, 182 Anaerobic column chromatography, 17-18/ Anaerobic transfer, 144 Anionic polymerization, 182 Apparatus design philosophy, 117 Arc lamp... 

Table II. Parts List for Pressure Reactor with Integral Pressure—Equalizing Addition Funnel...

In a typical reaction, a mixture of 16 g of chipped laminated particle board, 150 mL of ethanol, and 3 g of concentrated sulfuric acid was heated at 200 C for 30 minutes in a 300-mL Parr pressure reactor. The mixture was allowed to cool to room temperature. The product mixture was filtered with a Biichner funnel, and the charcoal residue was washed with ethanol and dried to give 5.4 g of charcoal. The filtrate was neutralized with sodium bicarbonate and distilled to recover the excess ethanol and the water, ethyl formate, and trace amounts of diethyl ether produced in the reaction. To extract the levulinate ester, diethyl ether was added to the residue from the distillation, which contained a small amount of ethanol. The insoluble portion of the distillation bottoms gave the resin product (3.3 g). The ether-soluble portion contained ethyl levulinate and a small amount of furfural. After the ether was stripped on a rotary evaporator, the residue (4.5 g) was vacuum-distilled to give ethyl levulinate (3.8 g) and impure furfural (0.4 g). 

The pyrolysis apparatus consists of a vertical, electrically-heated Vycor tube (25 mm. I.D.) packed with 6-mm. lengths of Pyrex tubing (10 mm. O.D.) and mounted in an electric furnace about 45 cm. long (Notes 1 and 2). Attached to the top is a 100-ml. dropping funnel with a pressure-equalizing side arm that has an inlet for nitrogen (Note 3). A thermocouple well inside the tube holds a movable thermocouple and extends to the bottom of the heated section (Note 4). The bottom of the reactor is fitted to a 500-ml. side-arm flask packed in ice. The side arm leads to tw o traps in series cooled in ice and to a final trap cooled in a bath of dry ice and acetone (Note 5). 

Gulf Research and Development Co. Two of the coals were processed in the Gulf continuous flow reactor, fed at the rate of about 1.5 kg coal/hr for 15-18 hrs. The third coal was processed in a conventional batch autoclave run. In all three runs, the coal was processed at about 400 °C and 3000 psi pressure of hydrogen using a proprietary catalyst. In the continuous runs, distillate from previous experiments was used as vehicle while in the autoclave experiment, partly hydrogenated phenanthrene was used. The vehicle-to-coal ratio was 2 1. In each case the reaction products were filtered on a steam-heated Buchner funnel. 

Two glass reactors for 50-150 psi gas/solution reactions are described. The first is a simple reactor with safety pressure release, sample withdrawal port, and quick connect hookup. The second incorporates a metal pressure-equalizing addition funnel for reactant additions to the pressurized reaction mixture. Plans and commercially—available parts lists for both designs are provided. 

A 1000-liter reactor is large, heavy, and stationary. Its situation and construction demand techniques little practiced in discovery or university research, call for modifications of methods or conditions used there, and forbid altogether some commonplace operations. For example, (1) the chemist using such a reactor cannot tilt it to pour its contents into a container more suitable for the next operation. One such operation, which entails washing with water a solution prepared with an organic solvent, must occur within the reactor, not in a separate funnel devoted to the procedure. As many successive operations as possible take place in the same vessel. Emptying the reactor requires that the contents flow freely, which lets them be pumped by suction, drained by gravity, or forced out by pressure. In any... 

The dinitrile (Smmoles) was charged in a dropping funnel. Then the autoclave was closed and purged repeatedly with nitrogen first then hydrogen. The reactor was heated under hydrogen pressure to the fixed reaction temperature. Dinitrile was introduced rapidly under stirring and this was considered as the zero time of the experiment. 

The pressure apparatus is first heated while the Ns stream passes throxigh. Then, 1.5-2 g. of [Co(NH3) s](N03)3 is admitted through a from a charging funnel and placed on the fritted-glass disk. The tube is then sealed at c. Next, a few mg. of Pt black and the required quantity of metallic K (3 moles of K per mole of [Co(NH3)e](N03)3 + 5% excess K) are placed in reactor b, and the tube is sealed at d. The stopcock on the Ns line is closed and the valve on the NH3 cylinder is opened. When the manometer in the NH3 line shows about 4 atm., the valve is closed and the NH3 is vented to the atmosphere by opening the vent stopcock. This purging process is repeated three times to displace the Ns from the apparatus. Then reactor b is immersed in ice-salt mixture, the valve on the NH3 cylinder fully opened, and NH3 allowed to condense in b until the latter is 3/4 full of liquid. Stopcock h is then closed and tube a is cooled so that NH3 distills from b into a. The hydrogen evolved in the reaction of K with NH3 is vented... 

Ultra high purity N2 (ca. 50 mL) was added after each sampling to restore pressure to the reactor. Each sample was cooled to room temperature in an ice bath, the pH measured and the sample extracted with 3x5 mL of dichloromethane (EM Science, Gibbstown, NJ) containing 500 ppm of 4-methylthiazole (Aldrich Chemical, Milwaukee, WI) as an internal standard in a 150 mL separatory funnel. The dichloromethane fraction was dried with anhydrous magnesium sulfate (Fisher Scientific, Fairlawn, NJ), filtered and evaporated to 0.5 to 1.0 mL volume under a stream of high purity nitrogen. 

The reactor system is pressurized by means of steam supplied from an electrically heated recirculation boiler, drawing water from the water volume of the pressurizer. The steam volume of the pressurizer is comparatively large and, together with its volume of saturated water, the reactor system can accommodate pressure and level variations that may occur during operational transients and accident situations. The pressurizer is connected to the reactor pool via funnels up into the steam volume, and to the reactor primary loop via open passages from the pressurizer "poor. 

A 100-mL Schlenk flask, magnetic stirrer, vacuum pump, low-temperature reactor, constant pressure funnel, safety glasses, laboratory coat, and protective gloves. 

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