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Volume 21, Issue 6
Displaying 1-9 of 9 articles from this issue
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Shoichiro YAMADA1963 Volume 21 Issue 6 Pages 413-424
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
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Kikuo KOEDA1963 Volume 21 Issue 6 Pages 425-434
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
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Heiun Ko1963 Volume 21 Issue 6 Pages 435-451
Published: June 01, 1963
Released on J-STAGE: March 01, 2011
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Liquid phase hydrogenation of DinitrotolueneTomohisa MURAKAMI1963 Volume 21 Issue 6 Pages 452-457
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSIn the liquid phase hydrogenation of dinitrotoluene (DNT) in 60% aqueous solution of tolylenediamine (TDA), the velocity of hydrogen absorption is proportional to the vapor-liquid contacting effect and the pressure of hydrogen, while the concentration of catalyst is proportional to a certain amount but has no relation beyond this amount. The effect of temp, is not so remarkable as in usual chemical reactions and also it has no relation with the concentration of DNT. Furthermore, the catalyst (Raney nickel) is rapidly poisoned when the concentration of DNT is high. The above result indicated that the hydrogenation of DNT should be made in such a way as to make a continuous feeding of it at a rate suitable for above reacting condition in order to reduce introduced DNT to TDA immediately. The solvent is unnecessary for the reaction by this method and DNT can be hydrogenated with high efficiency.View full abstractDownload PDF (778K) -
Phosgenation of Tolvlene diamineTomohisa MURAKAMI1963 Volume 21 Issue 6 Pages 458-462
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSReaction of amines and phosgene at low temp, for conversion of the amino group into carbamyl chloride and amine hydrochloride, and further reaction of this at high temp, with phosgene is known so-called Cold-Hot Method for synthesis of isocyanate. In case diamine such as TDA is used, a high molecular urea compound is formed by the wrong procedure of reacting condition and precipitated, so that the reaction with phosgene becomes difficult, resulting considerable decrease in the reaction velocity and yield. For successful operation of this reaction, it is necessary to make sufficient contact of phosgene with TDA in low temp. reacction in order to decrease the amount of unreacted TDA in the product and sufficient supply of phosgene in high temp, reaction. It is desirable to use solvents, such as ketones, esters and ethers, having high solubilizing power of low temp. reaction product. Also, chlorobenzene, dichlorobenzene, etc. could be used as the solvents by adding TDA solution into phosgene solution with vigorous stirring, in order to give finely dispersed particles of low temp, reaction product. The high temp, reaction is completed in 30 min at 130°c by sufficient introduction of phosgene in the low temp, reaction product thus obtained and the yield is high.View full abstractDownload PDF (602K) -
Syntheses of Hydroxy methyl acetophenone from Cresyl acetate.Takeshi YOSHINO, Ichiro KIJIMA, Michio SUGIURA, Toru SHOJI.1963 Volume 21 Issue 6 Pages 463-465
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSReactivity of phenol esters in the Fries reaction has been investigated by using titanium tetrachloride as a catalyst in the preceding experiment. This report deals with the Fries reaction of cresyl acetate and the yield of acetophenone, its reacting condition, time and temp., the amount of catalyst and solvent, etc. have been investigated. Syntheses of additive products of m- and p-acetates and titanium tetrachloride were carried out at first, their decomposition temp. and the synthesis of acetophenone from the additives have been investigated. m-Cresyl acetates yielded o- and p-compounds, while p-cresyl acetate yielded o-compound only. In each case, the max. yield was 90% and 70%, respectively, at the decomposition temp. of additive products. The change of reaction time in these temp, ranges showed great effect in its yield. In case of m-cresyl acetate, the yield of p-compound became higher when aluminium chloride was used as a catalyst.View full abstractDownload PDF (351K) -
Oxidation of p-Carboxybenzophenone by PeracidsAkio NOGUCHI, Hirozô KUBOTA, Kôsaku HONNA1963 Volume 21 Issue 6 Pages 466-472
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
JOURNAL FREE ACCESSOxidation of p-carboxybenzophenone (1) with peracetic acid in glacial acetic acid or acetic anhydride as a solvent gave a monophenyl acid terephalate (2) and it was discovered that simultaneous syntheses of terephthalic acid and phenol were possible from hydrolysis of (2). The kinds of peracids and solvents used for the oxidation, the amount and time of pouring of hydrogen peroxide, the concentration of sulfuric acid, and the temp. of reaction have been investigated and the best condition for the reaction was proceeded as follows : To 1 mole (1), 13.3 moles of glacial acetic acid and 500 cc conc sulfuric acid, as a catalyst are added, and then the solution at 40°c is treated dropwise with 1.03 moles of 30% hydrogen peroxide in 30 min, stirred for 6 hr at this temp. The product (2) is hydrolyzed as usual with aqueous sodium hydroxide solution and the separation of the products by suitable means yields 86.5% of terephthalic acid with purity 97.6% (Hasen no. 65) and 83, 8% of phenolView full abstractDownload PDF (816K) -
Nobuhiko KUROKI1963 Volume 21 Issue 6 Pages 473-484
Published: June 01, 1963
Released on J-STAGE: July 05, 2011
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Toshinao OKITSU1963 Volume 21 Issue 6 Pages 485-489
Published: June 01, 1963
Released on J-STAGE: June 28, 2010
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