Bergwerksverband Gmbh

Sigri Elektrographit Gmbh

Georg Kolling

Ingo Romey

Kurt Handrick

Hellmut Kokot

Clemens Linden

Carl Kroger

Karl K Knoblauch

Harald Juntgen

Jurgen Klein

Harald Tillmanns

Gerhard Pietzka

Hans-Jurgen Schroter

Horst Schumacher

Gunter Droll, Jr

Fritz Mensch

Paul Kiedel

Process of preparing .beta.-isopropylnaphthalene substantially free of corresponding .alpha.-isomer, in yields amounting to 90% and more by a continuous two-stage process comprising (1) alkylating naphthalene with propylene at a temperature of about 150.degree.-280.degree. C. under a pressure of 5 to 30 atm in the presence of a phosphoric acid catalyst supported on a SiO.sub.2 carrier and using a mol ratio of 1/5 to 1/20 mol propylene to 1 mol naphthalene to isopropylate 45 to 65% of the naphthalene and form a mixture of .alpha.- and .beta.-isopropylnaphthalene and then without separating off the unreacted naphthalene, (2) heating the isomeric mixture from stage (1) in the presence of a phosphoric acid catalyst supported on SiO.sub.2, to a temperature of 180.degree.-280.degree. C. under an inert gas pressure of 5 to 30 atm until no further .beta.-isopropylnaphthalene is formed and recovering said .beta.-isopropylnaphthalene from the isomerization mixture.

Preparation of .beta.-isopropylnaphthalene

A method for production of anthracene from phenanthrene is disclosed. Phenanthrene is hydrogenated at a nickel on a carrier catalyst at temperatures from about 140.degree. C. to 170.degree. C. under a pressure of from about 10 to 30 bar by gradual addition of hydrogen. The hydrogenation product is separated by distillation into sym.-octahydrophenanthrene and asym.-octahydrophenanthrene. The sym.-octahydrophenanthrene is isomerized in the presence of methylene chloride as a solvent and of aluminum chloride as a catalyst at a temperature from about -30.degree. to +5.degree. C. to sym.-octahydroanthracene. The sym.-octahydroanthracene is dehydrogenated at a chromium oxide-aluminum oxide catalyst at temperatures from about 450.degree. to 550.degree. C. to anthracene. The resulting anthracene is obtained with high yield and is very pure after a single recrystallization step.

Anthracene production from phenanthrene

In a method for the production of hydrocarbon resins based upon pyrolysates through cationic polymerization of the pyrolyzate in the presence of Friedel-Crafts catalysts and solvents at temperatures between -40.degree. and +60.degree. C., tetralin and/or tetralin derivatives are pyrolysed at 660.degree.-710.degree. C., preferably at 675.degree.-690.degree. C., in the presence of 1-10 mol, preferably 3-7 mol, vaporous water per mole tetralin or tetralin derivative with a dwell time of 1-2 seconds; the pyrolyzate is distilled to free it of high boiling (tarry) portions; and the unsaturated compounds contained in the distillate are polymerized in known manner. Styrene formed during the pyrolysis is preferably removed through distillation before the polymerization. The hydrocarbon mixture regenerated with the separation of the resins formed through polymerization are hydrogenated to tetralin and/or tetralin derivatives and again pyrolyzed.

Method for the production of hydrocarbon resins

Coal tar pitch is liquified at temperature of from about 135.degree. C. to 280.degree. C. The liquid coal tar pitch is filtered through a sieve with apertures from about 100 to 220 .mu.m and with a closed surface area of at least 75 percent of the total sieve surface under pressures of from about 2 to 10 bar until a filter cake of a height of from about 40 to 80 mm forms above the sieve for separating ash, soot and quinoline insoluble particles from the liquid. Then the filtrate obtained is subjected to a coking process. The needle cokes resulting in accordance with the invention provide excellent materials for the production of graphite electrodes.

Method for the production of needle coke

Manufacture of isotropic coke by first selecting as feed material tar from low temperature carbonization with a hydrogen content above 5.5%, a carbon content less than 88% and a softening point above 60.degree. C., filtering the tar to remove solid particles, and heating the filtrate to a temperature between about 900.degree. C. and 1300.degree. C. to form an isotropic coke.

Method of producing an isotropic coke

Process for making indole by subjecting 1,2,3,4-tetrahydroquinoline to a thermal decomposition at a reaction temperature of about 650.degree. to 750.degree. C. in a reactor filled with a substantially inert material and in the presence of steam. The starting product for this process is easily available and can easily be obtained by chemical reaction and the process itself has a high yield.

Process for making indole

Coal-containing shaped bodies are made by intimately mixing particulate coal with 10 to 30 percent by weight of a polymer. The mixture is shaped by subjecting it to a pressure between about 295 and 3430 newtons per square centimeter. Shaping takes place within a temperature range of 100.degree. to 250.degree. C. The shaped bodies have high compressive and bending strengths and can be precisely dimensioned.

Coal-containing shaped bodies and process for making the same

A process for the manufacture of anthraquinone, in which o-benzyl-toluene is oxidized with air or an oxygen-containing gas in an acetic acid solution in the presence of cobalt, manganese and bromine salts as catalysts, to which solution sufficient acetic anhydride is added to bind the reaction water, thereby keeping the acid concentration constant. The crude o-benzoyl-benzoic acid is then esterified with methanol, the methyl ester distilled from the reaction mixture and heated with concentrated sulfuric acid to yield anthraquinone in good yield and of a high degree of purity.

Catalytic oxidative process for the manufacture of anthraquinone from

A process for the manufacture of anthraquinones in which o-benzyl-toluene is first oxidized with 25 to 50 weight-% nitric acid at atmospheric pressure and moderate temperatures, and then further oxidized with a more dilute nitric acid at elevated temperatures and pressures to yield crude o-benzoyl-benzoic acid. The crude product is then esterified with methanol, the methyl ester distilled and, when necessary, recrystallized, and heated with concentrated sulfuric acid to yield anthraquinone in high yield and of a high degree of purity.

Nitric acid process for the manufacture of anthraquinone from

A carbonaceous adsorbent in the form of a shaped body which has been heated to about 400 to 1400.degree. C in an inert atmosphere is composed essentially of a mixture of finely divided carbonaceous material of a grain size below 50 and up to below 100 microns with a binder composed of about 1 to 20% by weight of a natural or synthetic elastomer and about 1 to 15% by weight of a thermoplastic material. The adsorbent is made by subjecting the mixture to a shaping step followed by heating to a temperature of about 400.degree. to 1400.degree. C in an inert atmosphere which step may be followed by an activation of the carbonaceous material.

Carbonaceous adsorbents and process for making same

Coal-tar pitch is heated to a temperature which is at least 100.degree. C above its softening point but below its decomposition temperature and is mixed with a filter aid, such as kieselghur or activated carbon prior to filtering the pitch at at least the preheat temperature so as to remove ashes, soot and heavy metals therefrom. The thus-purified pitch is then coked. In this manner, it is possible to obtain high-quality, anisotropic acicular coke which is readily convertible into graphite.

Process for the production of coke from pitch

Pitch having a Kramer-Sarnow softening point between 70.degree. and 190.degree. C is heated to a temperature in the range of 40.degree. to 100.degree. C above the softening point thereof. There is thus obtained a molten mass having non-molten particles distributed therein. A filtering operation under a pressure greater than atmospheric pressure is carried out to remove the particles from the molten mass. The molten mass may then be treated in different ways. According to one embodiment, the molten mass is held at a temperature between 280.degree. and 350.degree. C to distill off low molecular weight components of the pitch and the resulting product is thereafter shaped by extrusion to the form of strands. According to another embodiment, the molten mass is cooled, ground to particulate form and contacted with an aliphatic solvent having a boiling point between 60.degree. and 70.degree. C. This solvent dissolves a portion of the ground mass and, after separation of the solvent from the residue, the latter is heated to a molten state and thereafter extruded into the form of strands. In either embodiment, the previously mentioned filtering operation provides for a greater homogeneity of the strands since the non-molten particles, which could form a second phase, are substantially completely eliminated. In both embodiments, the strands obtained are dusted with finely divided activated carbon which has been impregnated with a liquid oxidizing agent. The dusted strands are oxidized in an oxidizing atmosphere at temperatures between 300.degree. and 400.degree. C. The oxidation increases the melt-resistance of the strands. The oxidized strands are next carbonized, the increased melt-resistance thereof preventing melting of the strands during the carbonizing treatment. If desired, the strands may also be graphitized. The method described enables carbon-containing or graphite-containing strands suitable for many applications to be produced in a much shorter time than was possible heretofore.

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Essen, Germany

Georg Kolling