Chemical Engineering Commons^™

The Preparation Of 3,4-Diaminopyridine, Emil John Fencl

Theses

The preparation of 3,4-diamincpyridine from pyridine was investigated, but found to be of little synthetic value because of the low yield obtained on the rearrangement of 4-nitraminopyridine to 3-nitro 4-aminopyridine. In attempt to nitrate nicotinamide-N-oxide resulted in the isolation of nicotinic acid-N-oxide. Attempts to nitrate nicotinic acid-N-oxide were unsuccessful. Attempts to oxidize 3-methylpyridine-N-oxide and 4-nitro-3-methylpyridine were unsuccessful. The nitration of 3-methylpyridine-N-oxide led to the isolation of 2-nitro-5-methylpyridine, which has not previously been reported as a by-product of that reaction.

Ammonia Catalized Phenol Formaldehyde Resins, Murlin Charles Ehrgott

Theses

The literature on ammonia-catalyzed phenol-formaldehyde resins is reviewed and critical comparisons are made of the manner in which the ammonia-catalyzed resins differ from both the alkali- and acid-catalyzed resins.

Intermediate products formea during the initial stapes of the ammonia-catalyzed phenol-formaldehyde reactions, as reported in the literature, are tabulated and % N contents are calculated.

Experimental determinations of N content of resins with molar ratios of 1:1.25 phenol to formaldehyde with ammonia at 0.2, 0.5, and 1.0 moles per mole of phenol, show that at the 0.2 molar ratio of ammonia, all the N enters into the resin and remains during …

Heat Transfer Coefficients In An Agitated Vessel Using Verticle-Tube Baffles, Edward Joseph Barrasso

Theses

Data are presented to show the effect of impeller speed, impeller type, and fluid properties on the forced-convection film coefficient of heat transfer for verticle tubes in a cylindrical vessel. A generalized equation to predict the film coefficient of heat transfer on the outside of verticle tubes in an agitated vessel for both cooling and heating is also presented. This equation may be used to estimate the necessary areas of heat transfer for verticle tubes in an agitated vessel within the degree of accuracy required from most engineering calculations.

This study was the first initiated to develop an equation to …

Electrodeposition Of Cellulose And Carboxy-Methylcellulose, Charles Edward Driesens Jr.

Theses

The previous work done by Frank Cozzarelli on the eleotrodeposition of cellulose from a sodium zincate-urea-cellulose system has been verified, except that zinc was found to deposit on the cathode at all voltages and current densities within the range of the optimum conditions for deposition. The optimum conditions are: voltage - 1.10 to 1.28 volts; current density 0.13 to 1.10 amperes/square foot; electrode material - copper. Current efficiencies range from 0.80 to 5.53%.

A chelate-like complex formed from the sodium zincate and urea which couples with the cellulose has been proposed as a possible explaination of the mechanism governing the …

Activity Coefficients Of Gases In Binary Mixtures, John Gressler Engleman

Theses

The theory and usefulness of vapor phase activity coefficients have been developed. The equations, charts and calculation procedures to be used for the three methods are included with a set of sample calculations in their most convenient form.

Activity coefficients for 236 experimental points have been calculated by the three methods for both components of tour binary gaseous systems. These systems are Argon - Ethylene (36 points), Hydrogen - Nitrogen (32 points), Methane - Ethane (112 points) and Methane - n Butane (56 points). Wide ranges of pressure, temperature and mol fraction are included.

The % deviations of calculated from …

Transesterification Of Alkyl Borates, Garry Gustav Eichmann

Theses

An attempt was made to prepare pure methyl borate by an ester interchange using a high-boiling alkyl borate in combination with methyl benzoate or methyl phthalate. The product, assumed to be methyl borate, boiled at about 70°C., which is 5° higher than the expected boiling point, and analyzed at 88 to 95%.

Various catalysts, such as hydrochloric acid, sodium methoxide, p-toluene sulfonic acid, aluminum isopropoxide, and aluminum chloride, were tried before magnesium-aluminum ethoxide was chosen as the best catalyst for this particular tranesterification reaction.

The Fatty Acid Alkanolamide Reaction, Julius Galender

Theses

An alkanolamide detergent can be formed by the condensation of coconut fatty acid and diethanolamine. A great many factors can influence this formation. It is shown that varying the molar ratio of amine to acid, results in a change in the fraction of acid converted. It similarly affects the molar quantities of amine converted. Molar conversion of acid or amine is dependent upon the type of atmosphere in the reaction; more acid is converted when a nitrogen sweep is employed than when it is not used. However, proportionately more amine is converted, when a nitrogen sweep is not used. When …

Power Requirements In Pigment Comminution, Joseph Timothy Gildersleeve

Theses

The results of this work prove that the relation between total work and surface area developed in the wet grinding of pigments is an exponential function. The following equations were experimentally determined for the pigments studied:

For Zinc Oxide; P = .090 (Δs)1.05

For Titanium Dioxide: P = .086 (Δs)1.072

For Calcium Carbonate: P = .107 (Δs)0.98

This work shows that in the grinding of sub-sieve size pigments the Rittinger and Bond theories which state that surface area developed is directly proportional to total work, are not valid and cannot be applied.

It is also shown in another plot that …

Composting Coffee Waste, Lawrence James Hickey

Theses

Disposal of waste, and specifically organic waste, has become a serious problem in such industries as the canning, meat-packing, dairy and other food producing industries. Recently, with the introduction of instant coffee powder, this particular industry now has a waste disposal problem with the resultant coffee residue. Composting or biologically decomposing this waste to yield an organic fertilizer is one of the many ways to solve this problem.

There are no papers in the literature concerning composting of coffee waste and only one paper (65) is available covering studies of high rate composting of garbage and refuse. It is known …

Heat Transfer Coefficients Of Condensing Vapors, Charles Rocco Lipuma, Earl Adolph Nirmaier

Theses

The film coefficients of heat transfer for vapors condensing on a single horizontal tube have been measured for methyl, i-propyl, and n-butyl alcohols. The equipment used was specifically designed for these studies, and represents an improvement over that used by other investigators. The data collected were analyzed usingmodified Wilson method which is based on a rigorous theoretical analysis.

It has been found that the condensing film coefficients for methyl and i-propyl alcohols vary with the heat duty. This is to be expected from the analysis mentioned above. Me variation was found for n-butyl alcohol.

The observed values of the heat …

The Condensation Of Vapors From Gas-Vapor Mixtures, Stanley Anthony Mruk, William Charles Kraemer

Theses

Superheated mixtures of cyclohexane vapor and nitrogen gas were passed at various rates downward through a single tube condenser with the cooling water flowing countercurrently in an annular space outside the condenser.

The method of Colburn and Rougen for the design of cooler-condensers was applied and the calculated condenser lengths are compared to the experimental length.

Relatively good agreement with the design method was found for cases where there was little or no streamline flow of the gas-vapor mixture in the condenser. With increasing amounts of streamline flow* the design method tends to be increasingly conservative.

The Three Phase System N-Hexane - Aniline - Water, Charles S. Potosnak

Theses

This is a study of the three phase system - n-Hexane Aniline - Water at 50° Centigrade. The data obtained, coupled with data previously established at 36° Centigrade is used to predict a means of recovering aniline from 3-5% aqueous solutions by scrubbing with n-hexane.

Thermodynamic Properties Of Trimethylamine, John Bernard Riley

Theses

The thermodynamic properties of trimethylamine have been evaluated at temperatures from 32°F to 600°F and from the saturation pressure to 2000 lb/in² based on available experimental data. An equation relating the pressure, volume and temperature of the system has been derived for the range in which experimental data were available and it was used to evaluate the thermodynamic properties in this range. Values for pressure, volume, temperature, enthalpy and entropy have been presented in the form of tables and graphs.

Effect Of Concentration On The Mass Transfer Coefficient In The Liquid Film, Marvin Baker Schaffer, Philip Major Pomerantz

Theses

The effect of liquid concentration on the resistance to mass transfer across the liquid film is studied for an acetone-methyl isobutyl ketone-air system in a packed tower. The liquid film resistance is computed by measuring the overall resistance for various concentrations and subtracting the gas film resistance. The gas film resistance is determined at the same liquid and gas rates by measurements on the pure components.

In the theory developed to handle the calculations, it is assumed that the interface temperatures are the wet-bulb temperatures based on a dynamic equilibrium. This supposition is supported experimentally at a liquid rate of …

A Study Of The Functional Stability Of Sunscreen Compounds, Jesse Howard Starkman

Theses

Previous work reported in literature, indicates that commercial sunscreen compounds were subject to breakdown on exposure to ultraviolet radiation with consequent change in their functional efficiencies.

These findings ware retested under conditions more closely approximating actual usage.

A new method of evaluation which closely correlates to actual experience in large scale usage, was applied. This method provides, from simple spectral data, a reliable index of physiological efficiency of the sunscreen compound. As a result, twelve commercial sunscreen compounds were exposed to ultraviolet radiation for varying periods. Analysis indicated that, contrary to the previous reports, no significant Changes in physiological efficiency …

Correlation Of Curtis And Gullett Equation For Viscosity Of Non-Newtonian Suspensions And Franks And Rinaldi Equation For Heat Transfer Coefficients, Irene S. Wisla, John L. Kukowski

Theses

Curtis and Gullett (7) developed an equation correlating the effect of velocity, concentration and particle size on apparent viscosity of non-Newtonian water slurries.

μ/μ_w=1.02(AK/GC)^.105

The object of this paper was to determine the validity of using the viscosity, as determined by the Curtis-GulLett (7) equation, in predicting the heat transfer coefficient of non-Newtonian fluids, where the suspending medium is something other than pure water . The authors used various concentrations of sugar solutions as the dispersion medium, for the slurries.

A dimensionless equation resembling the flittusBoelter equation with modified exponents and additional dimensionless groups has been developed …

A Study Of The Partial Oxidation Of Monosubstituted-P-Xylenes, Frederick John Honold

Theses

In the oxidation of 2-nitro-p-xylene (I) using alkaline potassium permanganate, the only product isolated was 2-nitro-terephthalic acid (II). Approximately half of the starting material was oxidized. The other half remained as unreacted starting material.

The chromium trioxide oxidation of 2-nitro-p-xylene (I) in glacial acetic acid, using sulfuric acid as a catalyst, yielded only 3-nitro-p-toluic acid (III).

The chromium trioxide oxidations, of 2-N-acetylamino-p-xylens (IV) with and without sulfuric acid catalyst, yielded no oxidation products which could be identified. About half of the starting material was recovered in each case.

In a low temperature alkaline potassium permanganate oxidation of 2-N-acetyIamino-p-xylene a small …

Intermediates For P-Acetamidocinnamic Ester Synthesis, William Grayson Fix

Theses

After a review of the various methods found in the literature, a series of reactions were selected which were reported to have good yields.

Using p-nitrotoluene as a starting material, a simultaneous oxidation and reduction with sodium polysulfide was investigated as a means of making p-aminobenzaldehyde. Experimental procedures and yields were reported, and improved methods of recovery were described.

Using p-aminobenzaldehyde from the first reaction, a condensation with malonic acid, in pyridine-piperidine medium, was investigated as a means of preparing p-aminocinnamic acid.

A recommended procedure was described, and some suggestions were made concerning the completion of the synthesis of p-acetamidocinnamic …

Vapor-Liquid Equilibrium Data And Distillation Packing Evaluation At High Vacuum, Edward Joseph Lasch

Theses

Vapor pressure date and vapor-liquid equilibria date at 1-30 m.m. pressure are presented for benzyl alcohol and benzyl-n-butyl ether system. Activity coefficients for the system are symetrical, the Margules constants ere A_1-2 = A_2-1= .301. HETP values observed at a condenser pressure of 1 m.m. for 1/4" and 3/4" Berl saddles, 1" Intalox saddles, Fibre Glass Combination packings # 076 and # 476, and a Knitted Wire Mesh pecking are presented as a function of the mass throughput and column pressure drop. At a condenser pressure of 1 m.m. the pressure drop per foot in terms of …

Graphical Correlation Of Pressure Drop And Temperature Drop To Friction And Velocity For Adiabatic Flow Of Compressible Fluids, Andrew Anthony Giacobbe

Theses

Problems involving adiabatic flow of compressible fluids in horizontal conduits of constant cross-section usually require tedious trial and error solutions. Although several somewhat simplified methods have been developed, most of these methods are not ideally suited for problems involving flow between two sections of a conduit.

The graphical solutions presented in this paper, relating pressure and temperature ratios to friction and initial Mach numbers, have been developed specifically for flow between sections of a conduit. Use of the graphs requires only the knowledge of initial conditions and determination of the friction factor.

Initial velocities from 30% to 70% of the …

The Sulfonation Of Some Aromatic Compounds Using Sulfuric Acid In The Presence Of Thionyl Chloride, Paul Juergens

Theses

The rate of reaction in the sulfonation of some aromatic compounds with sulfuric acid was increased by the presence of thionyl chloride which, by reacting with the water of formation, effectively maintained the concentration of sulfuric acid above the level at which sulfonation can occur. The thionyl chloride had no measurable effect on the formation of isomers.

The sulfonstion reactions studied included those of toluene, naphthalene, bromobenzene, ortho-bromotoluene, and chlorobenzene.

The Heat Of Mixing Of Diactone Alcohol And Water At 25 C, Frederic Miller Konrad

Theses

A calorimeter of twin design with auxiliary apparatus was built for measuring the heat of mixing with a maximum error of ± 1.0%. Reliability of the apparatus was tested with the benzene-methanol system and gave results comparable to those of other investigators with apparatus of different design.

The heat of mixing of diacetone alcohol and water was measured at 25°C over the entire concentration range. A peak value of 238 cal/mole solution was obtained at 0.67 mole fraction water the mixing of two moles water with one of diacetone alcohol.

Specific heat of diacetone alcohol-water mixtures was also measured at …

Variation Of Thickness Of Hard Anodic Films, Alphons Raymond O'Konski

Theses

An investigation was made of the effects of varying processing conditions on the thickness of anodic films produced by the Martin Hard Coat (4) process on commercially pure aluminum and nine aluminum alloys.

This study was conducted to provide sufficient data for designing coating thicknesses on aircraft accessory parts that would conform to the close tolerances maintained in the course of manufacture of precision components. Coating thicknesses up to 0.0051 in. were obtained. Changes in electrolyte strength, temperature of the bath, alloy composition, and current density were made to see their effect on the thickness of the film and growth …

The Recovery Of Krypton From Dilute Gas Mixtures By Elution Techniques, David Graham Brown

Theses

An analytical method has been empirically developed for the analysis of dilute inorganio inert gas mixtures.

The method is based on a combined sorption-elution technique which makes possible the resolving of complex inert gas mixtures into their constituents.

Particularly the recovery of krypton from dilute gas mixtures was accomplished. Recovery efficiencies were as high as ninety-eight percent, while the average krypton purity was better than ninety-nine percent.

Heat Transfer Coefficients For Condensing Vapors On A Horizontal Tube, Maurice Edward Brown, Rodwin Edwin Gulick

Theses

Film coefficients of heat transfer for vapors condensing on a smooth horizontal tube have been experimentally determined by many investigators. The so-called Thermocouple Method and the Wilson Method, have been used and generally accepted as the two methods for determining these film coefficients. A number of different organic vapors have been studied on various condensing surfaces. Nusselt has also developed a theoretical equation,

hN = 0.725 4√k_f³ρf²λg/D_oμfΔtcf

for evaluating the film coefficients of vapors condensing on hori?zontal tubes.

The earlier investigators have shown that theoretical values, hN do not check with experimentally determined …

Bis Phenol Epichlorohydrin Condensate Modification Of Alkyd Resins, Raymond Francis Carmody

Theses

A method is given for the modification of alkyd resin systems with Bis-Phanol Epichlorohydrin Condensates.

The properties of the modified alkyd resins are evaluated using similar unmodified alkyd resins as reference.

A theory of linear esterification is postulated.

The Analogy Between Heat And Mass Transfer In Packed Beds, Jasper Joseph Correnti

Theses

An operation which recurs in many branches of chemical engineering is that in which a fluid - gas or liquid - is passed through a bed of granular solids for the purpose of removing from, or adding something to the fluid (or both). In the oil and sugar industries, oils or syrups are passed through beds of adsorbents to remove impurities causing color and other undesireable effects. In the recovery of volatile solvents, air charged with solvent vapor is passed over solid adsorbents. In leaching, liquids are passed through beds of solids to remove some constituent of the solids. In …

The Effect Of Reduced Pressure On Variables In Distillation, Joseph Peter Cummins

Theses

To determine the effects of reduced pressure on pressure drop and holdup in distillations seven different liquids were distilled at varying rates at atmospheric pressure and under vacuum at pressures down to 50 mm Hg, using protruded stainless steel packing. Pressure drop and holdup were found to vary exponentially with masste at each pressure. At constant mass rate pressure drop was higher for decreased head pressure. Use of material of higher molecular weight led to lower pressure drop at same rate and pressure. Greatest effect of pressure on pressure drop was observed below 300 mm Hg. Liquid holdup was not …

Heat Capacity Ratios Calculated From The Benedict-Webb-Rubin Equation State, Edward George Delaney

Theses

The ratio of the isobaric heat capacity to the constant volume heat capacity has been calculated over a range of temperatures and pressures for the following hydrocarbons: methane, ethylene, ethane, propane, and n-butane. Graphs and tables of calculated data are presented showing the effect of temperature and pressure on the ratio of the heat capacities for these compounds.

The deviations of the heat capacities from ideal gas behavior were calculated by previous investigators from an equation based on the Benedict-Webb-Rubin equation of state, Experimental data were used to evaluate the heat capacities of the ideal gases, and were used together …

Continuous Chlorosulfonation Of Benzene : I. Phase Relations, Henry Benjamin Lange

Theses

This work presents liquid-liquid equilibria data on a system suitable for continuous chlorosulfonation of benzene. Complete information is presented for the ternary, chlorosulfonic acid - sulfuric acid - carbon tetrachloride. A partial investigation of the ternary systems, chlorosulfonic acid - sulfuric acid - benzenesulfonyl chloride; chlorosulfonic acid - carbon tetrachloride - benzenesulfonyl chloride; and the quaternary system, carbon tetrachloride - benzenesulfonyl chloride sulfuric acid - chlorosulfonic acid is also presented.