Reaction kettles

A typical chem manufg operation is the production of trinitrotoluene — TNT, the dominant mil expl. It involves the manuf of huge quantities of nitric and sulfuric acids, from sulfur and ammonia, in chem plants exactly similar to those which make nitric and sulfuric acids in the civilian economy. Mixed nitric and sulfuric acid is then combined with liq toluene in a series of reaction kettles... 

Into a 1-L three-necked glass reaction kettle equipped with a mechanical stiner, nitrogen inlet tube, and a distillation head connected to a condenser are... 

The checker found it expedient to carry on the reaction in a 2-1. Pyrex reaction kettle (Coming 6947), the large closure making the initial mixing of the solid reactant and the removal of the product much simpler. 

Synthesis of Urethane Modified Acrylics and Acrylic Modified Urethanes. 1) Synthesis of PBH. Into a reaction kettle equipped with a nitrogen inlet, stirrer, reflux condenser, and an addition funnel charged 500g of xylene. The xylene was heated to reflux and a mixture of 375g butyImethacrylate (BMA), 125g of 2-... 

Synthesis of PBHI. Into a reaction kettle, equipped with nitrogen inlet, stirrer, reflux condenser, and thermometer were charged 464g of PBH, I7lg of... 

A reaction kettle was charged with the step 1 product (7.5 mol) and /V-methyl-ethano-lamine (8.25 mol) and then treated with a 28% methanol solution of sodium methox-ide (0.075 mol). This mixture was heated to 70°C for 20 hours while distilling off methanol under reduced pressure. Thereafter, the mixture was treated with acetic acid (5 g) and then concentrated. After distillation 1146 g of product was isolated as a pale yellow transparent liquid with a 96% purity having a bp of 135°C 2 mmHg. 

A reaction kettle equipped with mechanical stirrer was placed in a glove box filled with nitrogen and heated to 120°C for 1 hour to remove moisture. The reactor was then charged with glycolide (200 g), y-caprolactone (200 g), 0.27 ml dodecanol, 700 ml of xylene, and 1.12 ml of stannous octoate and where glycolide component was added over four portions in 2-hour intervals. The mixture was then stirred at 120°C for 90 hours and the product isolated after dissolving in chloroform and precipitated in methanol. 2... 

The oiganic and aqueous phases are prepared in separate tanks before transferring to the reaction kettle. In the manufacture of a styrenic copolymer, predetermined amounts of styrene (1) and divinylbenzene (2) are mixed together in the oiganic phase tank. Styrene is the principal constituent, and is usually about 90—95 wt % of the formulation. The other 5—10% is DVB. It is required to link chains of linear polystyrene together as polymerization proceeds. DVB is referred to as a cross-linker. Without it, functionalized polystyrene would be much too soluble to perform as an ion-exchange resin. Ethylene—methacrylate [97-90-5], and to a lesser degree trivinylbenzene [1522-25-2], are occasionally used as substitutes for DVB. 

The essential parts of the apparatus are shown in Fig. 8. The 4-1. reaction kettle, A, has a flanged top with four female standard-taper openings, one (34/45) centrally... 

The center joint, B, of the reaction kettle is fitted with a chimney, C, in the top of which is a rubber stopper, D. Two tungsten rods, E, about 6 mm. in diameter, pass through this stopper and support a tungsten filament, F, which is capable of being heated to 1000 to 1100°. The... 

The reaction is continued until the tetrachloride no longer refluxes freely down the sides of the vessel. The filament is then turned off, and the whole reaction kettle is heated to drive off the residual tetrachloride, which tends to be absorbed in the cake of solid trichloride. To condense and remove the tetrachloride, a still head and horizontal condenser are substituted for the reflux condenser. 

The processing equipment (reaction kettle and blending tank) used for unsaturated polyesters can also be used for manufacturing alkyd resins. 

The apparatus used for the in vitro dissolution studies consisted of a two-piece 1 L reaction kettle (Fisher Scientific Co. Cat. No. 11-847B). The top cover has four openings, three of which were stoppered and the center one left open for the stirrer shaft. The exterior of both the top and bottom pieces were painted black to allow use with light-sensitive drugs. Stirring was provided by a three-blade, polyethylene stirrer... 

Adding aqueous formaldehyde solution to a reaction kettle can also make Hexamine. Then ammonia gas (in a 3 2 formaldehyde/ammonia mole ratio) is added. During the addition of the reactants, the temperature is maintained at about 20 to 30°C. The reaction mixture is then fed to a vacuum evaporator where it is maintained at a temperature between 30 and 50X1 and at a pH of 7 to 8252. 

Despite the chemical diversity of the several hundred structures representing herbicidal activity, most reactions of herbicides fall within only a limited number of mechanistic types oxidation, reduction, nucleophilic displacements (such as hydrolysis), eliminations, and additions. "Herbicides", after all, are more-or-less ordinary chemicals, and their principal transformations in the environment are fundamentally no different from those in laboratory glassware. Figure 2 illustrates three typical examples which have received their share of classical laboratory study—the alkaline hydrolysis of a carboxylic ester (in this case, an ester of 2,4-dichlorophenoxyacetic acid, IX), the cycloaddition of an alcohol to an olefin (as in the acetylene, VI), and the 3-elimination of a dithiocarbamate which provides the usual synthetic route to an isothiocyanate (conversion of an N.N-dimethylcarbamic acid salt, XI, to methyl isothiocyanate). Allow the starting materials herbicidal action (which they have), give them names such as "2,4-D ester" or "pronamide" or "Vapam", and let soil form the walls of an outdoor reaction kettle the reactions and products remain the same. 

The terpolymerizations described were carried out by a continuous feed method, unless stated otherwise, where both the monomer mixture and the initiator were added together continuously to the reaction kettle (18). The variables studied were (1) effects of initiators with different half-lives, (2) effects of variations in temperature, and (3) effects of variations in concentrations of initiators. Attempts were also made to study the extent of heterogeneity in the products. 

Resin Preparation. All phenolic resins were prepared in the laboratory. Resin preparations were replicated one time. To prepare each resin, all phenol and water were placed in a reaction kettle. The formaldehyde was added in three steps 1) total formaldehyde less 1 mole of formaldehyde was added at the beginning 2) the balance was divided into two equal parts (i.e., 0.5 mole each), one of which was added 1 hour after the reaction began and 3) the remainder of formaldehyde was added 20 minutes later. The sodium hydroxide was added as catalyst in four steps (i.e., four equal parts at 10-minute intervals). To initiate the reaction, the mixture was heated and maintained at 75 °C. All reactions were terminated at the end of 100 minutes. Gel time, pH, viscosity, solid content, and specific gravity were determined. The general conditions for resin preparation were ... 

Fig. 35. Reaction kettle (Samesreuther). The kettle is equipped with external heating or cooling coils. The coils are mounted on copper supports (b) which conduct heat to or from the kettle. This heating system is quite different from that used in the Frederking apparatus (Fig. 34). If the kettle wears out, the heating system can be used for a new kettle. These kettles are very useful, e.g., for suffonations in which varying heating and cooling must be used (see p. 211, H acid).

Closed reaction kettles, as a rule, have their stirrers built in, usually of the anchor-type which reach nearly to the bottom and sides of the kettle. 

In a reaction kettle constructed as shown in Figure 36 (page 333), a mixture of 138 grams (1.0 mole) of p-nitroaniline and 225 grams (2.5 moles) of dry oxalic acid (anhydrous ) is heated with good stirring at 110°C. The two compounds should be finely pulverized and intimately mixed beforehand, and six steel balls of 25 mm. diameter should... 

Fig. 29. Cast iron reaction kettle with stirrer for use at pressures up to 2 atm. weight, 12 kg. The oil bath is made of copper.

A reaction kettle was charged with polyesterdiol (0.5 mol M 1000 daltons prepared from isophthalic acid, adipic acid and hexanediol), polyethylene glycol (0.05 mol Mw= 1500 daltons), and dimethylolpropanoic acid (1.25 mol) dissolved in methyl ethyl ketone. The mixture was heated to 80°C. When the reaction was completed the... 

A reaction kettle was charged with propylene glycol monomethyl ether acetate (5.1 g) and propylene glycol monomethyl ether (3.4 g) and then heated to 80°C. This mixture was next treated dropwise with the Step 1 product (2.7 g), 3-hydroxyadamantane methacrylate (4.7 g), 2-methyl-2-adamantyl methacrylate (7.0 g), y-butyrolactone methacrylate (6.8 g), and the free radical initiator V-601. Thereafter the reaction proceeded for 2 hours at 80°C and was then cooled and poured into a 720 ml mixture of hexane containing 80 ml of EtOAc. The precipitate was collected, and 18 g of product were isolated having a Mw of 10,700 daltons with a polydispersity of 1.81. 

III) chloride from a freshly opened bottle is placed in the dropping funnel. The reaction kettle then is cooled by lowering it into the gallon Dewar containing a 1 1 mixture (by volume) of carbon tetrachloride and chloroform cooled to —78° with excess Dry Ice. 

A10.5.1.2 All glass test vessels must be carefiilly cleaned by standard laboratory practices, acid-cleaned (e.g. HCl) and subsequently rinsed with de-ionized water. The test vessel volume and configuration (one- or two-litre reaction kettles) should be sufficient to hold 1 or 2 / of aqueous medium without overflow during the agitation specified. If air buffering is used (tests carried out at pH 8), it is advised to increase the air buffering capacity of the medium by increasing the headspace/liquid ratio (e.g. 1 / medium in 2.8 / flasks). 

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